Is 6191 1971
Is 6191 1971
METHODS OF
MICRO-BIOLOGICAL COLOUR FASTNESS
AND MICROSCOPICAL TESTS FOR LEATHER
© Copyright 1984
INDIAN STANDARDS INSTITUTION
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
Gr 11 August 1972
IS : 6191 - 1971
Indian Standard
METHODS OF
MICRO-BIOLOGICAL COLOUR FASTNESS
AND MICROSCOPICAL TESTS FOR LEATHER
Leather Sectional Committee, CDC 16
Chairman Representing
DR Y. NAYUDAMMA Council of Scientific & Industrial Research
Members
SHRI R. K. AGARWAL Leather Research & Testing Laboratory ( Director
of Industries, Government of Uttar Pradesh ),
Kanpur
SHRI H. R. GADI ( Alternate )
SHRI M. BANERJEE College of Leather Technology ( Government of
West Bengal ), Calcutta
SHRI R. A. BHOTE Directorate of Marketing & Inspection (Agriculture),
Nagpur ( Ministry of Food, Agriculture,
Community Development & Cooperation )
SHRI T. G. BOSADE Ministry of Defence ( R & D )
SHRI O. P. DHAMIJA Export Inspection Council of India, Calcutta
SHRI V. N. SRIVASTAVA ( Alternate )
SHRI S. K. DUTTA Directorate General of Ordnance Factories
( Ministry of Defence )
SHRI A. S. BHATTACHARYA ( Alternate )
SHRI T. N. GANJWAR India Leather Corporation Ltd, Madras
SHRI J. GHOSH The State Trading Corporation of India Ltd,
New Delhi
SHRI A. K. SEN ( Alternate )
SHRI N. KANNAN Ministry of Defence ( DGI )
SHRI W. G. EDGAR ( Alternate )
SHRI P. U. K. MENON Gordon, Woodroffe & Co (Madras) Pvt Ltd,
Madras
SHRI G. P. MADHAVAN ( Alternate )
SHRI K. V. S. MURTHI Planning Commission, New Delhi
SHRI A. NAGAPPA CHETTIAR Leather Export Promotion Council, Madras
SHRI T. ABDUL WAHID ( Alternate )
SHRI S. NAGARAJAN Development Commissioner, Small Scale Industries,
New Delhi
SHRI NASIM IQBAL The Tanners' Federation of India, Kanpur
SHRI A. K. PRAMANICK Directorate General of Supplies & Disposals
( Inspection Wing ), New Delhi
SHRI A. T. BASAK ( Alternate )
SHRI S. RAJA The Tanner, Bombay
SHRI T. RAJAGOPAL RAO The Associated Tanners, Vizianagaram
( Continued on page 2 )
Members Representing
SHRI G. ROY CHAUDHURY Export Promotion Council for Finished Leather &
SHRI I. B. SARKAR ( Alternate ) Leather Manufactures, Kanpur
SHRI SANJOY SEN The National Tannery Co Ltd, Calcutta
SHRI J. SINHA ROY ( Alternate )
SHRI N. R. SARKAR Bata Shoe Co Pvt Ltd, Calcutta
SHRI V. LEITENEDORFER ( Alternate )
SHRI P. K. SARKAR Indian Leather Technologists' Association, Calcutta
SHRI P. R. SONDHI Kapurthala Northern India Tanneries Ltd,
Kapurthala
SHRI R. R. SONDHI ( Alternate )
SHRI R. THANJAN Directorate General of Technical Development,
New Delhi
SHRI R. S. GHOSH ( Alternate )
SHRI D. DAS GUPTA, Director General, ISI ( Ex-officio Member )
Director ( Chem )
Secretary
SHRI S. DAS GUPTA
Assistant Director (Chem), ISI
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IS : 6191 - 1971
CONTENTS
PAGE
... ... ... ... ...
0. FOREWORD 5
... ... ... ... ...
1. SCOPE . 6
2. TERMINOLOGY ... ... ... ... ... 6
3. SAMPLING LOCATION ... ... ... ... 7
4. QUALITYOF REAGENTS ... ... ... ... 7
5. TESTS . ... ... . ... . ... ... ... 7
PAGE
LF : 8 DETERMINATION OF FASTNESS OF COLOURED
LEATHER TO W A T E R SPOTTING ... ... 41
LF : 9 DETERMINATION OF FASTNESS TO RUBBING
( W E T AND DRY ) OF LIGHT LEATHERS ... 42
LF : 10 DETERMINATION OF COLOUR FASTNESS
RUBBING ( CROCKING T E S T ) ... ...TO 48
LF : 11 DETERMINATION OF FASTNESS OF COLOURED
LEATHER TO MARKING ... ... ... 49
LF : 12 DETERMINATION OF FASTNESS OF COLOURED
LEATHER TO WASHING ... ... ... 50
LF : 13 DETERMINATION OF THE COLOUR TRANSFER OF
LEATHER DURING WASHING ... ... 52
LF : 14 FASTNESS TO RUBBING OF LIGHT LEATHERS
WETTED FROM BACK WITH ORGANIC SOLVENTS 54
Indian Standard
METHODS OF
MICRO-BIOLOGICAL COLOUR FASTNESS
AND MICROSCOPICAL TESTS FOR LEATHER
0. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Institution
on 21 January 1971, after the draft finalized by the Leather Sectional
Committee had been approved by the Chemical Division Council.
0.2 This standard includes revisions of certain methods of test prescribed
in IS : 582-1954*, compiles all the methods prescribed in different material
specifications and adds several new methods based on the international
line of thinking and practice in the trade and export market.
0.3 In Section I, this standard prescribes test methods for assessing the
resistance of leather, hides and skins to mould growth. These methods
have been based on the methods developed and/or followed by the Central
Leather Research Institute, Adyar, Madras.
0.4 In Section II, various methods of test for determining the colour
fastness of the leather have been prescribed. These methods replace the
methods prescribed in 25 and 26 of IS : 582-1954*. By colour fastness is
meant the resistance of leather to the different agencies to which the
leather may be exposed during manufacture, storage and subsequent use.
Each method described in this section, concerns itself with colour fastness
of single agency. No consideration has been given for testing fastness to
succession of agencies, because of the complexity of the problem and since
the agencies of interest in a particular case and the order of application
varies quite often. The methods provide a common basis for testing and
reporting colour fastness. The conditions have been chosen to correspond
closely with treatments usually employed in manufacture and with condi-
tions of general use and storage. They have been kept as simple and
reproducible as possible. The fastness ratings should be interpreted
according to the particular needs of each user as it is not possible to
reproduce here all the conditions under which leathers are processed, used
or stored. The methods prescribed in this section are based broadly on
the methods adopted by Society of Leather Trades Chemists, UK, which
are based on the original methods evolved by the Society of Dyers and
Colourists, and the methods developed by the Shoe and Allied Trades
Research Association ( SATRA ).
*Methods of sampling and test for vegetable and chrome tanned leathers.
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IS : 6191 - 1971
0.5 In Section III, standard methods are given for the preparation of
microscopical slides by different techniques and staining them for study of
fibre structure, common defects and the grain pattern of hides, skins and
leather under a microscope. It is true that the microscopical methods of
assessment of leather cannot at present replace the conventional physical,
chemical and functional methods of test; nevertheless such methods provide
supplementary data which help in quick study of the fibre structure during
tanning operations and the pattern of grain structure and defects in
finished leather.
0.6 In the preparation of this standard considerable assistance has been
derived from the following publications:
ASTM STANDARD — Part 15-1966 Paper; packaging; cellulose;
casein; flexible barrier materials; leather. American Society for
Testing and Materials.
BS 3662 : 1962 Methods for the determination of the colour fastness
of leather, issued by British Standards Institution.
ALCA Methods of analysis. American Leather Chemists Associa-
tion, 1957.
Official methods of analysis. Society of Leather Trades' Chemists.
UK.
0.7 In reporting the results of a test or analysis made in accordance with
this standard, if the final value, observed or calculated, expressing the
result of a test or analysis, is to be rounded off, it shall be done in accor-
dance with IS : 2-1960*.
1. SCOPE
1.1 This standard prescribes various microbiological test methods in
Section I, colour fastness test methods in Section II and test methods for
the preparation of microscopical slides for assessment of leather, hides and
skins in Section III.
1.1.1 In the case of any inconsistency, between the methods of this
standard and those of the standards for the individual materials, the latter
shall prevail.
2. TERMINOLOGY
2.1 For the purpose of this standard, the definitions given in IS : 1640-
1960† shall apply.
*Rules for rounding off numerical values ( revised ).
†Glossary of terms related to hides, skins and leather.
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IS : 6191 - 1971
5. TESTS
5.1 Unless otherwise agreed to between the purchaser and the supplier,
normally tests shall be carried out within two months from the date of
receipt of the material by the purchaser.
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IS : 6191 - 1971
1. SCOPE
1.1 The method is intended for assessing the resistance offered by the
pickled pelt to mould growth by spore-swelling technique.
2. OUTLINE OF METHOD
2.1 Untreated as well as those pelts treated with agents to promote
resistance to mould are smeared with spore suspension of species found in
pickled pelt. With the assistance of untreated pelt, mould growth is
evaluated by examining the significant increase in the diameter of the
spores of the treated leather.
3. APPARATUS
3.1 Incubator — capable of maintaining temperature at 25 ± 1°C.
3.2 Microscope — fitted with ocular micrometer.
3.3 Petri Dishes
3.4 Slides — glass with cover
4. REAGENTS
4.1 Standard Spore Suspension — Use conidio spores of 7 days old
culture of Aspergillus niger on czapek slants.
4.2 Culture Medium — The following materials shall be used to prepare
the culture medium:
Saecharose 30 g
Sodium nitrate 2g
Dipotassium phosphate 1g
Magnesium sulphate 0.5 g
Potassium chloride 0.5 g
Ferrous sulphate 0.01 g
Agar 15 g
Water 1 000 ml
Heat to boiling, dissolve medium, distribute in tubes and sterilize by
autoclaving at 1.05 kg/km2 for 15 minutes.
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IS : 6191 - 1971
5. TEST PIECE
5.1 Cut two pieces each of 25 × 25 mm from both treated and untreated
pickled pelt.
6. PROCEDURE
6.1 Transfer one drop of the spore suspension to a slide and measure the
length and width of a spore at right angles to each other. Take the
average of the two readings to get the diameter of the spore. Measure the
diameter of specified number of spores in the same way using 5 fresh
mounts ( see Note below ). Place the test pieces ( see 5.1 ) on a glass slide
with the grain side up. Distribute uniformly with a micropipette 0.01 ml
standard spore suspension on each test piece. Rub the test pieces grain to
grain. Place these pieces on a glass slide supported on glass rods over
petri dishes containing moist filter paper. Close petri dishes and place
them under a bell jar and incubate at 25 ± 1°C for 48 hours. After
incubation, transfer the spores from pickled pelt to a microscopic slide by
touching the grain side of the incubated pelt by a drop of saline solution
placed on the slide. Apply a clean cover slip and measure the diameter of
36 or more spores in the same way again. Simultaneously carry out tests
with control test pieces cut from the untreated pelts.
NOTE 1 — In order to eliminate the possible bias in selecting the spores for measure-
ment, a mechanical stage is used. The slide should be mixed horizontally towards one
side and the first spore appearing in the outside field is measured followed by the next
spore appearing in the outside field. The procedure should be repeated till the required
number of spores are measured.
NOTE 2 — If the untreated control test pieces of pelt fail to show any significant
increase in the spore diameter or growth of mould, the test shall be considered incon-
clusive and the test should be repeated.
NOTE 3 — Since the basic distributions of the variables involved with regard to the
spore size of mould used here are not known satisfactorily, large number of spore
samples ( see Note 1 ) are measured.
NOTE 4 — The spores of the species of mould Aspergillus niger develop at very low pH
level obtained in pickled pelts in the absence of suitable fungicides.
NOTE 5 — The minimum number of spores for any test should be 36.
7. EVALUATION
7.1 Calculate the value Z according to the expression given below for each
set of diameter readings corresponding to either treated or untreated pelt:
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IS : 6191 - 1971
where
= mean of spore diameter readings ( x1, x2, , xn1 ) before
incubation,
y = mean of spore diameter readings ( y1, y2, , yn2 ) after
incubation,
n1 = number of spore diameter readings measured before
incubation,
n2 = number of spore diameter readings measured before
incubation, and
s' = refers to the standard deviation of the pooled samples and is
given by
7.1.1 For untreated pelt the value of Z less than or equal to 1.96 indi-
cates that the mould growth is insignificant and so the test shall be repeat-
ed with fresh culture of the test organism.
7.1.2 For treated pelt the value Z greater than 1.96 indicates that the
mould growth has been significant and therefore the skins have not been
treated adequately with the agents which promote resistance to the growth
of mould.
8. REPORT
8.1 The report shall indicate the following:
a) Number of test pieces tested;
b) The variations, if any, from the method;
c) The value of Z ( see 7.1 ); and
d) Number of spores taken into consideration for measuring the
diameter n ( see 6.1 ).
0. GENERAL
0.1 The procedure for the method of test to be followed shall be
determined by the end use of the leather, as well as by the type of fungi-
cide ( whether water soluble or not ), which may have been used in the
treatment of the leather.
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IS : 6191 - 1971
1. SCOPE
1.1 This method is intended for the determination of the resistance offered
by leather to the growth of moulds on it.
2. OUTLINE OF METHOD
2.1 Untreated leathers as well as leathers treated with agents to promote
mould resistance are smeared, sprayed or swabbed with mixed spore
suspension of species of mould found in tanned leathers and the resistance
of such leathers to the growth of mould is evaluated.
2.1.1 Conditions prescribed for preparation of specimens in this test
method correspond to the conditions to which leathers are subjected in use
and normal storage.
3. TEST PIECES
3.1 The test pieces shall be 50 × 10 mm rectangular pieces cut from
leather samples from the sampling position for physical testing of leather
( see 3.2.1 of IS : 5868-1970.* ).
4. PREPARATION OF TEST PIECES
4.1 Follow the procedure given in 4.1.1, 4.1.2 or 4.1.3 depending on the
nature and serverity of the condition to which the leather is subjected to in
use and/or storage.
4.1.1 Weigh test pieces, then leach by drumming for three hours in
about 30 times their weight of distilled water ( see IS : 1070-1960† ) at
27 ± 2°C. Then drain the leached test pieces, blot and inoculate.
4.1.2 Keep test pieces for seven days at 45 ± 2°C in an oven with
forced air circulation and leach by drumming for three hours in about
30 times their weight of water at 27 ± 2°C ( see IS : 196-1966‡ ). Then
drain and blot the leached test pieces.
4.1.3 Test the test pieces as received.
4.2 Control Test Piece — The control test piece shall be of the same
type of tannage and finish as the treated leather. For this, the same
manufacturer may supply a piece of untreated leather along with the
treated material. This may be avoided if one can obtain the same with-
out recourse to the manufacturer of treated leather, for this purpose.
NOTE — Inclusion of a control piece of same tannage helps in getting information on
the natural resistance of the leather to mould growth, depending upon the type of
tannage and whether the spores of the test organism are viable.
5. APPARATUS
5.1 Containers for Keeping Test Pieces — Any suitable glassware
which may be conveniently stoppered, namely, jars, desiccators, glass
tanks, etc, with greased covers to preclude loss of water vapour during the
test may be used. The vessel may contain water at the bottom or cotton
wool or clean sand previously saturated with boiling water. This is done
to obtain 100 percent relative humidity at approximately 30°C.
5.2 Incubator — capable of maintaining 30 ± 2°C and 95 to 100 per-
cent relative humidity.
5.3 Oven — with forced air circulation to maintain temperature of
45 ± 2°C.
6. REAGENTS
6.1 Standard Mixed Spore Suspension — Standard mixed spore sand
suspension ( see Note ) of the following cultures of species of moulds should
be used in the test:
Asperguills niger
Aspergillus flavus
Aspergillus terreus
Aspergillus mdulans
Faecilomyces varioti
Penicillium frequentans
Penicillium rubrum
Pericillium purpurogenum
With each batch of such a suspension a list showing the organisms
incorporated therein as well as the date prior to which the culture is to be
used shall be furnished.
NOTE — At present sand suspension of spore of species of moulds usually found in
tanned leathers are supplied by Central Leather Research Institute, Madras.
7. PROCEDURE
7.1 Take four treated test pieces ( see 4.1 ). Dampen with sufficient water
for about five minutes, smear, spray or swab with mixed spore suspension
and subsequently suspend them above a free water surface in a suitably
covered vessel as described in 5.1.
7.2 Viability Control — Simultaneously, tests shall be carried out with
control test pieces of leather not treated with fungicide. If this untreated
material fails to show any growth of the test organism, the test shall be
considered inconclusive and whole test be repeated.
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IS : 6191 - 1971
7.3 Incubation — Incubate the test pieces for 30 days at 30 ± 2°C and
95 to 100 percent relative humidity in the incubator ( see 5.2 ) or humidity
cabinet and keep in the dark.
7.4 Examine the test pieces at frequent intervals, at least once a week and
note the date of the first appearance of mould growth.
NOTE — The same vessel shall not be used for simultaneous testing of specimens
treated with different fungicides. Separate vessels shall be used for control pieces.
prescribed period, the test piece may have vigorous, moderate, slight or no
growth of mildew ( see 8.1 of LB : 2 ). Treat the test piece with fungicides
to such an extent that no growth of mildew is just observed in them; the
efficiency of the fungicide treatment is best judged by the performance of
the treated leather following the above procedure when subjected to
mildew growth test and improvement made till no growth is obtained.
Reckon it back to the actual area of the leather to be treated with
fungicide.
4. PROCEDURE
4.1 Soak 50 × 75 mm leather test piece, cut out from sampling portion
( see 3.2.1 of IS : 5868-1970* ) with occasional flexing for 2 hours in the
*Method of sampling for leather.
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IS : 6191 - 1971
*Methods for the determination of the colour fastness of leather, issued by the British
Standards Institution.
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IS : 6191 - 1971
fugitive, Standard No. 8 the most resistant and each standard being at
least twice as fast as the one below it. Thus, if it takes a year for
Standard No. 5 to fade under certain conditions, then the same amount of
fading will occur on Standard No. 4 in six months under the same condi-
tions, whereas about two years would be needed in the case of Standard
No. 6. It is known that certain of the standards possess some defects, but
they are the best at present available; the Society of Dyers and Colourists
is continuing its investigations into the problem.
1.5 It is necessary to ensure that different people testing the same leather
will cause it to become faded to the same extent before assessment against
the simultaneously faded standard. The ultimate users of coloured
leathers differ widely in what they consider to be 'faded articles' and,
therefore, patterns under test are faded to two different degrees which
adequately cover most opinions; these required degrees of fading are
defined by reference to a collection of standard patterns ( grey scale ) show-
ing different contrasts; fading to two degrees makes assessment more
reliable.
1.6 This general principle of assessing on the basis of moderate and
severe fading is complicated, however, by the fact that some patterns
undergo a slight change within the first few days — or even hours — of
exposure but do not change further for months or even years. These
slight changes are such that under normal conditions of use they would
seldom be observed. There are often changes in colour rather than true
fading, that is, destruction of colour, but in certain cases they become
important as the following example shows:
A handbag leather is exposed so as to produce a moderate degree of
fading and it is found that Standard No. 6 has faded to the same
extent; the general light fastness of the leather is therefore 6. A retailer
has a handbag of this leather in his window and on it a cardboard
ticket indicating the price. After a few days the ticket is removed and
careful examination reveals where it has been resting because the
surrounding leather has changed slightly on exposure to light.
The important factor about this slight change is that it is possible
only to detect the change when there is a sharp boundary between the
exposed and unexposed areas and these conditions rarely, if ever,
occur during normal use.
1.7 T h e retailer would, however, not expect leather of such good ???
fastness as No. 6 to be so affected during such a short exposure and this
standard has been designed so as to warn everyone when this may occur.
If such material were assessed at the first perceptible change in appea-
rance, the rating would be low, for example, 2. In order to indicate the
possibility of material of otherwise high-last fastness undergoing such a
slight initial change, therefore, this standard insists upon an additional
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IS : 6191 - 1971
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IS : 6191 - 1971
mercury-vapour lamps differ so much from daylight that their use in light
fastness testing is inadmissible. A Xenon arc, however, has an emission
spectrum very close to daylight, and if a suitable filter is placed between it
and the patterns which corrects the ultraviolet radiation to that occurring
in daylight, anomalies from the cause should not occur; the Xenon test
lamps made by Quarzilampen GmbH, Hanau, Germany, and the Model
60 lamps made by Atlas Electric Devices Co, Chicago, USA, are of this
type.
2.4.2 Differences in Effective Humidity — The light fastness of a pattern often
varies according to its moisture content during exposure, and this is govern-
ed by the humidity of the air in contact with the pattern, termed the
effective humidity. The effective humidity is a complex factor which takes
into account not only the relative humidity of the surrounding air, but
also its temperature, the surface temperature of the pattern and, in daylight
testing, the intensity of the light; full details of the importance of this factor
in light fastness testing have been published, but briefly it has been found
that the effective humidity is always lower than the relative humidity of
the surrounding air if the surface temperature of the pattern is higher than
the air temperature. Sunlight and the light sources used in fading lamps
cause surface heating, although in some lamps this is minimized by the
provision of a heat filter in the form of a glass-and-water or an infra-red
absorbing glass screen between the light source and the patterns.
2.5 In fading lamps, the effective humidity may be less than 5 percent in
some cases and over 80 percent in other cases. Lamps operating at an
effective humidity below 5 percent may give results up to two grades
higher than daylight ( assuming the average volume of daylight as 45 per-
cent ) whilst at 80 to 85 percent the results may be two grades lower,
depending on the humidity sensitiveness of the pattern.
2. TERMINOLOGY
2.1 For the purpose of this method, the following definitions shall apply.
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IS : 6191 - 1971
3.1.5 Actual scales used shall not deviate from the values specified in
Table 1 ( see 3.1.4 ) by more than the tolerance values specified in Table 2
for the corresponding numerical fastness ratings.
TABLE 2 TOLERANCES
*One NBS Unit is regarded by the American National Bureau of Standards as being
a colour difference of some commercial significance.
4. PROCEDURE
4.1 Place the control piece of leather and the treated piece of it side by
side ( without leaving any space between them ) in the same plane and
oriented in the same direction. Place the geometric grey scale nearby in the
same plane, the surrounding field being uniform grey of a brightness slightly
less than that of the darkest member of the scale. Illuminate the surfaces
with sky light or equivalent source of illumination of 540 lux or more, the
light being incident upon the surfaces at approximately 45° and the direc-
tion of viewing approximately perpendicular to the plane of the surfaces.
Compare visually the difference between the control piece and the treat-
ed test piece, with the differences represented by the scale. Assign to the
lot that number of the scale which corresponds to the difference between
the control piece and the treated test piece. If, however, the difference
between the control piece and the treated test piece lies between two of
the differences of the scale, assign to the lot an intermediate rating, for
example, 3-4 or 4-3 ( these ratings being identical ). Assign to the lot a
rating of 5 only if there is no difference between the treated test piece and
the control piece.
NOTE — The sky-light referred should be North sky-light in Northern Hemisphere or
South sky-light in Southern Hemisphere.
NOTE — In assessing change of colour, the overall difference between the control
piece and the treated test piece is the basis for evaluation, the character of the change in
colour whether in hue, depth, brightness or any combination of these, being not rated.
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IS : 6191 - 1971
(1) (2)
5 0
4 4
3 8
2 16
1 32
*One NBS Unit is regarded by the American National Bureau of Standards at being
a colour difference of some commercial significance.
3.2.4 Actual scales shall not deviate from the values specified in Table 1
by more than the tolerance values given in Table 2 for the corresponding
staining ratings.
TABLE 2 TOLERANCES
GRADE THEORETICAL (NBS TOLERANCES (NBS
UNITS*) UNITS*)
(1) (2) (3)
5 0 ± 0.2
4 4 ± 0.3
3 8 ± 0.5
2 16 ± 1.0
1 32 ± 2.0
*One NBS Unit is regarded by the American National Bureau of Standards as being
a colour difference of some commercial significance.
4. PROCEDURE
4.1 Place a piece of the unstained uncoloured material and the treated
piece of it side by side ( without leaving any space between them ) in the
same plane and oriented in the same direction. Place the geometric
staining scale nearby in the same plane, the surrounding field being
uniform grey of a brightness slightly less than that of the darkest member
of the geometric grey scale. Illuminate the surfaces with sky light or
equivalent source of illumination of 540 lux or more, the light being
incident upon the surfaces at approximately 45° and the direction of
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IS : 6191 - 1971
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IS : 6191 - 1971
3. SAMPLING
3.1 Samples to determine conformity of a lot of coloured leather to a
specification shall be drawn according to IS : 5868-1970*.
4. TEST PIECE
4.1 Cut an area of the leather not less than 1 × 6 cm, from the sample.
*NOTE — To facilitate handling, the test piece(s) and strips of standard patterns of
similar size may be mounted on a card in some such arrangement as indicated in Fig. 1
or Fig. 2.
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IS : 6191 - 1971
5. STANDARD PATTERNS
5.1 Patterns of blue wool cloth ranging in light fastness from rating No. 1
( very low light fastness ) to rating No. 8 ( very high light fastness ) and
dyed with the dyes listed as prescribed in Table 1 shall be used for this
test ( see Note below Table 1 ).
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IS : 6191 - 1971
NOTE — Sets of standard patterns of light fastness ratings No. 1 to 8 may be obtained
from ISI. They are specially dyed to match master set of standard patterns in colour
and in fading behaviour. It has been found that, when repeated dyeings for the dyed
standard patterns are made, the amount of dye required to match a previous lot is often
different from that originally used. The dyeing strengths would, therefore, be
misleading and they are intentionally, omitted from this list.
6. APPARATUS
6.1 For the purpose of this test, the following apparatus shall be used.
6.1.1 Exposure Rack — facing due South in the Northern Hemisphere,
( or due North in the Southern Hemisphere ) and sloping at an angle of
45°, placed in the open in a location such that shadows of surrounding
objects would not fall on the exposed test piece(s) or standard patterns;
the rack shall be covered with window glass to protect the test piece(s)
and standard patterns from the weather, the glass being not less than 5 cm
from the test piece(s) and shall be provided with adequate ventilation.
6.1.2 Geometric Grey Scale* — for evaluating change in colour ( see LF : 1 ).
6.1.3 Opaque Cover — an opaque cardboard or other thin opaque
material, for example, thin sheet aluminium or cardboard covered with
aluminium foil ( three pieces ).
7. PROCEDURE
7.1 For mounting and testing for light fastness, follow any one of the two
methods prescribed in 7.2 and 7.3.
*Available from Indian Standards Institution, New Delhi.
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IS : 6191 - 1971
7.2 Method 1
7.2.1 Mount the test piece and the standard patterns on a card and
arrange them as shown in Fig. 1. Place an opaque cover ( see AB in
Fig. 1 ) across the middle third of the test piece and the standard patterns.
Place the assembly in the exposure rack and expose it every day from sun
rise to sunset. Follow the effect of exposure by occasionally removing the
opaque cover and inspecting the test piece.
7.2.2 When a change in colour ( see Note 1 ) of the exposed portion of
the test piece is just perceived ( see Note 2 ), find the light fastness rating
number of the standard pattern showing a similar change. Provided this
rating number is No. 3 or lower, note it as the preliminary light fastness rat-
ing number of the test piece.
NOTE 1 — The term change in colour includes not only true fading, that is, destruc-
tion of dyes, but also changes in hue, depth, brightness or any combination of these
characteristics of colour. If the difference in colour is a change of hue or brightness,
this may be indicated by adding abbreviations, as follows, to the numerical fastness
rating:
Bl = Bluer R = Redder D = Duller
G = Greener Y = Yellower Br = Brighter
NOTE 2 — If the change b accompanied by a change in depth this may also be
indicated:
W = Weaker S = Stronger
Phototropic test pieces should be allowed to condition in dark at
room temperature for 2 hours before evaluating the change in colour.
7.2.3 Again expose and follow the effect of exposure until a change in
colour equal to the difference in colour between the two grey colour chips
of the Geometric Grey Scale ( see LF : 1 ) illustrating the numerical fastness
rating 4 occurs first on the exposed portion of either ( i ) the test piece, or
( i i ) the standard pattern of light fastness rating No. 7.
7.2.4 If (a) the change in colour of the exposed portion of the standard
pattern of light fastness rating No. 7 is equal to the difference in colour
between the two grey colour chips of the Geometric Grey Scale illustrating
the numerical fastness rating 4, and (b) the change in colour of the
exposed portion of the test piece is equal to or less than the difference
in colour between the two grey colour chips of the geometric grey scale
illustrating the numerical fastness rating 4, conclude the exposure and
remove the cover.
7.2.5 Compare the change in colour of the exposed portion of the test
piece with the changes in colour that may have occurred in the standard
patterns of light fastness ratings No. 7 and No. 8. Assign to the test piece
the light fastness rating number of the standard pattern which shows
similar change in colour, adding within brackets the preliminary fastness
rating number, determined as in 7.2.2.
29
IS : 6191 - 1971
NOTE — When a test piece has light fastness rating of 7 or higher, it would require
unduly long exposure to produce a change in colour equal to numerical fastness rating
3 of the geometric grey scale; moreover, this difference would be impossible to obtain
when the light fastness rating number it 8. Evaluations in the region of ratings No. 7
to No. 8 are, therefore, made when the change in colour produced on standard pattern
of light fastness rating No. 7 is equal to the numerical fastness rating 4 of the Geometric
Grey Scale, the time required to produce this change being alone enough to eliminate
any error which might result from inadequate exposure.
7.2.6 If (a) the change in colour of the exposed portion of the standard
pattern oflight fastness rating No. 7 is less than the difference in colour
between the two grey colour chips of the geometric grey scale illustrating
the numerical fastness rating 4, and (???) the change in colour of the exposed
portion of the test piece is equal to the difference in colour between the
two grey colour chips of the geometric grey scale illustrating the numerical
fastness rating 4, replace the cover AB in exactly the previous position,
cover the left hand third of the test piece and the standard patterns with
another opaque cover ( see CD in Fig. 1 ), expose the assembly and follow
the effect of exposure until the change in colour of the right hand exposed
portion of the test piece is equal to the difference illustrating the numerical
fastness rating 3 ( see Note under 7.2.5 ). Remove the two covers.
NOTE — The test piece would thus have two exposed areas instead of one obtained
in accordance with 7.2.3.
7.2.7 Compare the changes in colour of the two exposed portions of the
test piece with the changes in colour of the corresponding portions of each
standard pattern.
[Link] If the change in colour of the two exposed portions of the test
piece are equal to or greater than the changes in colour of the correspond-
ing portions of the standard pattern of light fastness rating No. 1, assign to
the test piece the light fastness rating number of that standard pattern.
[Link] If the change in colour of the two exposed portionsof the test
piece are exactly similar to the changes in colour of the corresponding
portions of any one of the standard patterns of ratings No. 2 to No. 8,
assign to the test piece the light fastness rating number of that standard
pattern.
[Link] If the change in colour of the right hand and left hand
exposed portions of the test piece are between the changes in colour of the
corresponding portions of a set of two standard patterns of consecutive
light fastness rating number, assign to the test piece an appropriate half
rating number indicating it with a hyphen between the light fastness
rating numbers of the two standard patterns.
Example:
A light fastness rating of 3-4 indicates that the test piece is not as
standard pattern of light fastness rating No. 4 but is faster than
standard pattern of light fastness rating No. 3 and that its final
rating is 3½.
30
IS : 6191 - 1971
[Link] If the changes in colour of the left hand and right hand
exposed portions of the test piece (a) are not equal to the changes in colour
of the corresponding portions of any of the standard patterns, or (b) do not
fall between the changes in colour of the corresponding portions of a set of
two-standard patterns of consecutive light fastness rating numbers, or
(c) the change in colour of the right hand exposed portion of the test piece
is equal to the change in colour of the corresponding portion of a standard
pattern, or falls between the changes in colour of the corresponding por-
tions of a set of two standard patterns of consecutive light fastness rating
numbers, and (d) the change in colour of the left hand exposed portion of
the test piece is equal to the change in colour of the corresponding portion
of a different standard pattern, or falls between the changes in colour of
the corresponding portions of a set of two standard patterns of consecutive
light fastness rating numbers, assign to the test piece a rating number
which is the arithmetical mean of the light fastness rating numbers of the
two standard patterns:
Example:
A light fastness rating of 5¾ ( 6 + indicates that the
light fastness rating number of the right hand exposed portion of
the test piece is 6 where as the light fastness rating number of
the left hand exposed portion is 5½ and that the final rating
number of the test piece is 5¾.
[Link] If the light fastness rating number of the test piece as
determined in [Link], [Link] or [Link] is 4 or higher assign to the piece its
light fastness rating number, but also add, within parentheses, its prelimi-
nary light fastness rating number, if any ( see 7.2.2 ).
Example:
A light fastness rating of 6(3) indicates that the test piece
changes very slightly in colour in the test when the standard
pattern of light fastness rating No. 3 just begins to fade, but that
on continuing the exposure the resistance to light of the test
piece is equal to that of the standard pattern of light fastness
rating No. 6.
7.3 Method 2
7.3.1 Mount the test pieces and the standard patterns on a card and
arrange them as shown in Fig. 2. Place an opaque cover ( see AB in
Fig. 2 ) on one quarter of the total length of each test piece and standard
pattern. Place the assembly in the exposure rack ( see 6.1 ) and expose it
for 24 hours per day. Follow the effect of exposure by occasionally
removing the cover and inspecting the standard patterns.
31
IS : 6191 - 1971
7.3.2 When a change in colour ( see Note 1 under 7.2.2 ) of the exposed
portion of the standard pattern of light fastness rating No. 3 is just
perceived, inspect any one of the test pieces ( see Note 2 under 7.2.2 ) and
compare the change in its colour, if any, with the changes in colour that
have occurred in the standard patterns of light fastness ratings No. 1, No. 2
and No. 3. Note the light fastness rating number of the standard pattern
showing a similar change and take it as the preliminary light fastness rat-
ing number of the test piece. Inspect the remaining test pieces, one by
one, and evaluate similarly the preliminary light fastness rating number, if
any, of each.
7.3.3 Replace the cover AB in exactly the previous position, again
expose and follow the effect of exposure until a change in colour of the
exposed portion of the standard pattern of light fastness rating No. 4 is just
perceived. Fix a second opaque cover CD in the position shown in Fig. 2,
overlapping the first cover.
7.3.4 Again expose and follow the effect of exposure until a change in
colour of the exposed portion of the standard pattern of light fastness rat-
ing No. 6 is just perceived; then fix a third cover EF in the position shown
in Fig. 2 the other two covers remaining in position. Expose and follow
the effect of exposure. Conclude the exposure just as soon as:
a) a change in colour equal to the difference in colour between the
two grey colour chips of the geometric grey scale illustrating the
numerical fastness rating 4, patterns on the exposed portion of the
standard pattern of light fastness rating No. 7,
OR
b) a change in colour equal to the difference in colour between the
two grey colour chips of the geometric grey scale illustrating the
numerical fastness rating 3, occurs on the most resistant test
piece.
7.3.5 Remove the three covers. Evaluate the light fastness rating
number of each of the test pieces, one by one, in the manner prescribed
in 7.3.6.
7.3.6 Compare the changes in colour of the three exposed portions of the
test piece with the changes in colour of the corresponding portions of each
standard pattern.
[Link] If the changes in colour of the three exposed portions of the
test piece are equal to or greater than the changes in colour of the
corresponding portions of any one of the standard pattern of light fastness
rating No. 1 assign to the test piece the light fastness rating number of
that standard pattern.
[Link] If the changes in colour of the three exposed portions of the
test piece are exactly similar to the changes in colour of the corresponding
32
IS : 6191 - 1971
33
IS : 6191 - 1971
3. SAMPLING — Same as 3 of LF : 3.
4. TEST PIECE — Same as 4 of LF : 3.
5. STANDARD PATTERNS
5.1 Same as 5.1 of LF : 3.
5.2 The humidity test control of red azoic dyed cotton cloth shall be
used.
NOTE — The humidity test control may be prepared by impregnating bleached
mercerized poplin with 4 g/1 Brenthol AN (CI Azoic Coupling Component 4) and
developing with 20 g/1 Brentamine Fast Scarlet R. Salt ( CI Azoic Diazo Component
13 ). The above humidity test control may be obtained from ISI.
6. APPARATUS
6.1 Light Source — Xenon arc lamp of correlated colour temperature
5 500° to 6 500° K.
6.2 Filter — A filter to be placed between the light source and the
assembly of test specimen(s) and standard patterns so that the ultraviolet
spectrum is steadily reduced, becoming zero at 310 to 320 mμ. Window
glass may be used as filter.
6.3 Opaque Cardboard or Thin Opaque Material — such as thin
sheet aluminium or cardboard covered with aluminium foil.
6.4 Geometric Grey Scale — for assessing the change in colour ( see
LF : 1 ).
7. EXPOSURE CONDITIONS
7.1 The test pieces are exposed in a well ventilated exposure chamber.
7.1.1 Normal Conditions
[Link] Moderate effective humidity — Light fastness of the humidity test
control 5, black-panel temperature Max 45°C.
7.1.2 Extreme Conditions — For testing the sensitivity of specimens to
humidity, the following extreme conditions are useful.
a) Low effective humidity — Light fastness of the humidity test control
6-7, black-panel temperature Max 60°C.
b) High effective humidity — Light fastness of the humidity test control
3, black-panel temperature Max 40°C.
34
IS : 6191 - 1971
8. PROCEDURE
8.1 Humidity Control — Exposed partially covered strips of the humidity
test control and standard patterns simultaneously until a contrast is
produced on the humidity test control equal to Grade 4 on the grey scale.
Assess the light fastness of the humidity test control and, if necessary,
adjust the controls on the lamp to give the selected exposure conditions
( see 7.1.1 and 7.1.2 ).
8.2 Mounting and Testing of Test Pieces — Expose the test piece(s)
and the standard patterns simultaneously under the conditions enumerated
in 7 in such a manner and for such times as are necessary to evaluate fully
the light fastness of each test piece relative to that of the standard patterns,
by successively covering the test piece(s) and exposed standard patterns
throughout the test duration.
8.2.1 For mounting the testing the test piece(s) follow any one of the
procedure prescribed in 7.2 and 7.3 of LF : 3.
8.2.2 If test pieces larger than the standards were exposed, a mask of a
neutral grey colour (approximately Munsell N/6) should be used in
assessment which covers the surplus area of the specimens leaving an area
equal to that of the standards open for comparative evaluation.
35
IS : 6191 - 1971
3. APPARATUS
3.1 A device incorporating the following features is required:
a) A copper member ( referred to as the bit ), weighing not less than
113 g with a polished chromium plated face 25.40 ± 1.27 mm
square, and with its other surfaces lagged with heat insulating
material.
b) Means for heating the bit progressively up to a maximum tempe-
rature of 270° C ( for example, an electrical resistance heating
element ). Means of switching the heat source on and off, or
otherwise controlling it.
c) Means for raising and lowering the bit and for bringing its face
into contact with the test piece, in a horizontal plane with a
uniformly distributed pressure of 1.36 ± 0.05 kg.
d) A hinged support, with an insulated face, on which the face of
the bit can be rested during heating and which can be moved
aside to enable the bit to be lowered into the test piece.
e) A platform not less than 38 mm square to receive the test piece.
To assist in obtaining uniform pressure the platform is centrally
mounted so as to tilt freely in all directions.
f) Means for measuring the temperature of the bit.
NOTE 1 — The apparatus shown in Fig. 1 provides the features in a convenient manner.
It is obtainable from the Shoe and Allied Trades Research Association, Satra House,
Rockingham Road, Kettering, Northampton.
NOTE 2 — A suitable thermometer has a 44.5 mm diameter dial and 50.8 mm stem.
The thermometer stem should be within the bit. At intervals of time the accuracy of
the scale reading should be checked with a standard mercury in glass thermometer.
NOTE 3 — If desired, the temperature of bit may be controlled by inserting a
thermostatic device in the heater circuit. This enables the bit temperature to held
steady ( within the tolerance limits ) at each temperature in turn, and is, therefore,
particularly convenient if several samples are to be tested in succession.
3.2 Geometric Grey Scale — ( see 3.1 of LF : 1 ).
3.3 Watch — Capable of being read to l/5th second.
4. TEST PIECE
4.1 Cut a strip of the leather approximately 115 × 36 mm. This permits
tests at three temperatures with sufficient space between the test areas.
5. CONDITIONING OF TEST PIECE
5.1 Condition test pieces to an atmosphere at 27 ± 2°C and 65 ± 2 per-
cent relative humidity ( see IS : 196-1966* ).
*Atmospheric conditions for testing ( revised ).
36
IS : 6191 - 1971
6. PROCEDURE
6.1 Apply a thin coat of anti-stick release agent* to the face of the bit, as
and when necessary to prevent sticking. Turn on the heat with the bit
resting on the insulating support, and place the test specimen on the
platform beneath the face of the bit, with the side which is to be tested
uppermost. When the temperature has reached about 20°C above the
temperature at which the test is to be done ( that is, approximately 170°C )
turn off the heat and when the temperature of the bit has fallen to
150 ± 3°C, move the insulating support aside and lower the face into
contact with the test area at the prescribed pressure. Start the stop
watch at the instant of contact. Raise the bit from the test specimen
after five seconds.
6.2 Repeat the test successively at 200 ± 4°C and 250 ± 5°C each test
being carried out on a fresh area of the specimen ( see Note 1 ). Allow the
test specimen to cool and condition for four hours in the standard atmos-
phere. Then compare the tested areas with the untreated leather. If the
*Releasil emulsion 66 which if commercially available in UK is suitable.
37
IS : 6191 - 1971
appearance of the leather has changed, polish the tested areas lightly, using
a clean soft cloth ( see Note 2 ) and a little Carnauba Wax Emulsion ( see
Note 3 ) if the grain has been tested or brush with a suede brush if a suede
has been tested. Assess the change in colour between the tested areas and
untreated leather using the grey scale.
NOTE 1 — If appropriate, other temperatures of test may be used.
NOTE 2 — A suitable cloth for polishing the leather is the cloth used for cleaning
rifle-barrels known as 'four by two'. A fresh area of the cloth should be used for each
test area of the leather.
NOTE 3 — The wax emulsion is made as follows:
30 g fatty grey carnauba wax
9 g oleic acid
6 g morpholine
are melted together with stirring and when blended, 25 ml of water at the boil is
slowly added with rapid stirring and the mixture is made up to 300 g. The emulsion
is stirred until cool and is then ready for use.
7. REPORT
7.1 Report the following:
a) The side of the specimen tested;
b) Temperature of test; and
c) For each temperature of test, (1) the observed contrast grading,
with a description of the nature of the change of colour, (2) any
other effects of the heat treatment, that is, fusing or breaking up
of the finish or loss of gloss.
3. APPARATUS
3.1 Cotton or Wool Textile Pieces — Two pieces, uncoloured, each
10 × 5 cm. Undyed cloth, if not otherwise specified, be of plain weave
of medium weight and free from finishes, residual chemicals and damaged
fibres. Cotton or linen should be bleached. Other materials shall be
cleaned to their usual degree of whiteness without bleaching.
3.2 Geometric Grey Scales* — same as 3.1 of LF : 1.
3.3 Geometric Staining Scale* — same as 3.2 of LF : 2.
3.4 Jar
3.5 Shaker — mechanically operated, for tumbling the jar at 30 to 60
rev/min.
4. REAGENTS
4.1 Solvent — Either of the following solvents shall be used.
4.1.1 Petroleum Hydrocarbon — Grade 145/205 of IS : 1745-1966† is
suitable.
4.1.2 Tetrachloroethylene
4.1.3 Trichloroethylene — ( see IS : 245 - 1962‡ ).
5. TEST PIECE
5.1 Cut a test piece, 10 × 5 cm from the air-dry leather to be tested.
Place the test piece between the two pieces of uncoloured material
( see 3.1 ). Make a composite specimen by sewing together along the
edges.
6. PROCEDURE
6.1 Place the composite specimen in the jar, cover with the specified
solvent ( see 4.1 ) at a liquor ratio of 25 ml solvent per 1 g weight of test-
piece. Close the jar and tumble at 30 to 60 rev/min for 1 hour at room
temperature. Take the composite test-piece from the jar, squeeze lightly
between clean pieces of filter paper to remove excess solvent, and dry by
suspending in air at room temperature. Assess the change in colour of the
test-piece and the staining of the uncoloured material with the appropriate
Grey Scales.
*Available from Indian Standards Institution, New Delhi.
†Specification for petroleum hydrocarbon solvents ( first revision ).
‡Specification for trichloroethylene, technical ( revised ).
39
IS : 6191 - 1971
7. REPORT
7.1 Report the solvent used, the numerical ratings for the colour change
of each side of the test-piece and the numerical ratings for the staining
of each piece of the specified uncoloured material.
4.1.1 Adjust the pH to 8.0 ± 0.1 with 0.1 N sodium hydroxide solution.
5. TEST PIECE
5.1 Cut a test piece 5 × 4 cm from the leather to be tested. Place the
test piece between two pieces of uncoloured material ( see 3.4 ) so that an
area of 5 × 1 cm of the uncoloured material is not in contact with the test-
piece and sew along the common 5 cm side to form a composite test piece.
NOTE — The method of preparing the composite test-piece ensures that an area of
uncoloured material remains practically unstained and this considerably facilitates
assessment of staining where this occurs.
6. PROCEDURE
6.1 Lay out the composite test-piece smooth in a flat-bottomed dish and
cover with the solution at a liquor ratio of 50 : 1. Place a glass plate on
the test piece and press evenly and lightly with the fingers to remove the
air bubbles. Allow to stand for 30 minutes at room temperature. Pour
off the solution without removing the glass plate, and allow the composite
test piece to remain under the plate for four hours at 37 ± 2°C. Sepa-
rate the test piece and the uncoloured material and dry them apart in air
at room temperature. Assess the changes in colour of each side of the test
piece and the pieces of uncoloured material with the Grey Scales.
7. REPORT
7.1 Report the numerical ratings for the colour change of each side of the
test piece and numerical rating for the staining of each piece of the
specified uncoloured material.
3. APPARATUS
3.1 Geometric Grey Scale* — same as 3.1 of LF : 1.
3.2 Pipette or Dropper — to deliver approximately 0.15 ml of water.
4. TEST PIECE
4.1 Cut a test piece of 10 × 5 cm approximately from the leather, to be
tested.
5. PROCEDURE
5.1 Place two drops ( approximately 0.15 ml ) of distilled water on the test
piece about 5 cm apart. After 30 minutes remove the residual water ( if
any ) of one drop by gently blotting with filter paper and observe the
physical effects. After standing 16 hours assess the change in colour of the
leather which has been spotted with the second drop with the grey scale;
subject the leather to a light manual treatment ( see Note ) and again
assess the change in colour with Grey Scale.
NOTE 1 — The physical effects which may be observed and should be reported
include swelling and loss of lustre. To detect these it may be necessary to tilt the
leather in all directions during observation and the magnitude of the effect should be
described by using one of the following terms — slight, moderate, or severe.
NOTE 2 — The type of manual treatment is that normally applied by the user, that
is, case and upper leathers should be slightly polished with a wax polish, gloving and
clothing leathers should be lightly staked, and suede leathers should be lightly brushed.
6. REPORT
6.1 Report the following:
a) Surface of the leather tested;
b) Any physical effects observed after 30 minutes; and
c) Numerical rating for the change in colour after standing 16 h
before and after manual treatment.
42
IS : 6191 - 1971
2. OUTLINE OF METHOD
2.1 The test-piece is rubbed with a revolving felt pad, and the number of
revolutions of the pad required to produce certain effects is measured.
3. APPARATUS
3.1 Fastness Testing Machine — The instrument consists of the follow-
ing features.
3.1.1 A horizontal platform to clamp the test piece.
3.1.2 A means of holding a 25.4-mm diameter circular felt pad against
the test piece under fixed loads of 0.73 kg and 2.5 kg including the weight
of the spindle and rotating the pad at 150 ± .5 rev/min.
3.1.3 Means to count the number of revolutions of the pad.
NOTE — A suitable machine conforming to the requirements, as shown in Fig. 1 may
be obtained from the Shoe and Allied Trades Research Association, Satra House,
Rockingham Road, Kettering, Northampton.
3.2 Felt Pads — 25.4 mm outside diameter, 3.16 mm inside diameter and
6.35 mm thick, medium soft, white felt.
3.3 Geometric Grey Scale* — same as 3.1 of LF : 1.
3.4 Geometric Staining Scale* — same as 3.2 of LF : 2.
4. TEST PIECE
4.1 The platform of the machine is so designed that pieces of leather of
any size may be placed on it. Shoes and other made-up articles may also
be tested.
5. PROCEDURE
5.1 For Wet Rubbing
5.1.1 Immerse the standard felt pads in boiling water, and allow to cool
to room temperature. Adjust the weight of each wet pad by squeezing out
water or adding cold water until it lies between 2.9 and 3.2 g immediately
before using. Pads shall not be kept in water for more than 24 h. Clamp
the leather test piece on the test piece platform of the machine and place
730 g weight on the platform at the top of the vertical shaft. Press a wet
felt pad on the three spikes at the bottom of the vertical shaft, lower the
pad on to the test piece, and immediately switch on the motor. After
eight revolutions of the pad, raise this from the leather, and switch off the
motor. Move the test piece so that a fresh area is below the pad, change
the pad for a new one, and repeat the test, giving 16 revolutions. Repeat
this procedure giving successively 32, 64, 128, 256, 512 and 1 024
revolutions.
*Available from Indian Standards Institution, New Delhi.
43
IS : 6191 - 1971
44
All dimensions in millimetres.
FIG. 1 APPARATUS FOR TESTING FASTNESS TO RUBBING
IS : 6191 - 1971
5.1.2 Dry the leather ( see Note 1 ) and arrange the tested areas in
sequence. When necessary to restore the appearance of the leather, apply
a little wax emulsion ( see Note 3 ) to the tested area, allow to dry thoroughly
and polish with a clean soft cloth ( see Note 2 ). Examine the tested areas,
and decide which is the first in numerical order of rubs, to show in its most
affected part ( normally the periphery ) contrast of appearance with the
surrounding leather equivalent to or greater than that given by Grade 4
on the Grey Scale for assessing change in colour. Assess the contrast bet-
ween the tested area which has been given 1 024 revolutions of the pad,
and the surrounding leather, using the Grey Scale. If this contrast is
equivalent to or greater than Grade 1, then decide which tested area is the
first in numerical order of rubs to show a contrast of this grade.
NOTE 1 — A hair dryer is convenient for drying the leather quickly taking care that
it is not overheated.
NOTE 2 — A suitable cloth for polishing the leather is the cloth used for cleaning
rifle barrels — known as 'four by two'. A fresh area of the cloth should be used for
each test area of the leather.
NOTE 3 — The wax emulsion is made as follows:
30 g fatty grey carnauba wax
9 g oleic acid
6 g morpholine
are melted together with stirring and when blended, 25 ml water at the boil is
slowly added with rapid stirring and the mixture is made up to 300 g. The emulsion
is stirred until cool and is then ready for use.
5.1.3 Express the results as (1) number of revolutions required to cause
a contrast of Grade 4 and a description of the nature of the change;
(2) number of revolutions required to cause a contrast of Grade 1 ( if this
is 1 024 or less ); (3) contrast grading after 1 024 revolutions and a
description of the nature of the change ( see Note below ):
NOTE — Typical results may be expressed as:
(1) 64 weaker ( 2 ) > 1 024 ( 3 ) Grade 2 darker
or ( 1 ) 256 greener (2) 1 024 ( 3 ) Grade 4 greener and
weaker
or ( l ) 32 weaker (2) 256 ( 3 ) Grade 1 weaker
5.2 For Transfer of Colour on Wet Rubbing
5.2.1 Place the pads, stained side uppermost; on a sheet of plate glass
and allow to dry at room temperature. Cut each in half along a diameter,
and allow to dry at room temperature. Cut each in half along a dia-
meter, and arrange in sequence on a black card, with half of a clean unused
pad beside each, the cut diameters coinciding. Examine the pads, and
decide which is the first in numerical order of rubs, to show a contrast of
appearance with the unused pads, equivalent to or greater than that
45
IS : 6191 - 1971
given by Grade 4 on the Grey Scale for assessing staining. Assess the
contrast between the pad which has been given 1 024 revolutions, and the
unused pads, using the Grey Scale. If this contrast is equivalent to or
greater than Grade I, then decide which test pad is the first in numerical
order of rubs to show a contrast of this Grade.
5.2.2 Express the results as: (1) number of revolutions required to cause
a change in colour of the pad equivalent to Grade 4, (2) number of
revolutions required to cause a change in colour of the pad equivalent to
Grade 1 ( if this is 1 024 or less ), (3) contrast grading after 1 024
revolutions.
5.3 For Dry Rubbing (Normal Test)
5.3.1 Clamp the leather test piece on the test piece platform of the
machine and place the 2.5-kg weight on the platform at the top of the
vertical shaft. Press one of the standard felt pads on to the three spikes at
the bottom of the vertical shaft, lower the pad on to the test piece and
switch on the motor. After 32 revolutions of the pad, raise this from the
leather and switch off the motor. Move the test piece so that a fresh area
is below the pad, change the pad for a new one and repeat the test giving
64 revolutions. Repeat this procedure giving successively 128, 256, 512
and 1 024 revolutions, and if desired 2 048 revolutions also.
5.3.2 Arrange the tested areas in sequence and polish them lightly using
a clean soft cloth and a little carnauba wax emulsion ( see 5.1.2 ) when
necessary to restore the appearance of the leather. Examine the tested
areas, and decide which is the first in numerical order of rubs, to show in
its most affected part ( normally the periphery ), a contrast of appearance
with the surrounding leather, equivalent to or greater than that given by
Grade 4 on the standard Grey Scale for assessing change in colour. Assess
the contrast between the tested area which has been given 1 024 revolu-
tions of the pad, and the surrounding leather using the Grey Scale. If this
contrast is equivalent to or greater than Grade 1, then decide which tested
area is the first in numerical order of rubs to show a contrast in this
Grade.
5.3.3 Express the results as: (1) number of revolutions required to cause
a contrast of Grade 4, and a description of the nature of the change,
(2) number of revolutions required to cause a contrast of Grade 1 ( if this
is 1 024 or less ), (3) contrast grading after 1 024 revolutions ( if this is less
marked than Grade 1 ) and a description of the nature of the change.
5.4 For Dry Rubbing ( Modified Form of Test for Finishes Which
Smear on Rubbing ) — Under the standard conditions of test given
in 5.3.1 some finishes which soften at moderate temperatures are found to
smear and pick up small fibres of the felt owing to the raise in temperature.
46
IS : 6191 - 1971
If this occurs, the fact shall be recorded, and the test procedure modified
as follows.
5.4.1 In order to determine the fastness to dry rubbing in conditions
where heat build-up does not occur, the procedure of 5.3.1 shall be repeat-
ed for these leathers but, in every test, allowing the finish adequate time to
cool after every N revolutions, N being decided by trial and error so that
smearing or other damages due to heat softening does not occur ( see
Note ).
NOTE — Trials on various leathers with thermoplastic finishes suggest that the follow-
ing procedure is usually, but not invariably, successful in avoiding smearing. If in the
normal procedure of 5.3 smearing is found to occur first at n revolutions, then when
testing as 5.4 use N = n/2 revolutions between cooling periods. The cooling periods
should be of 0.5 min and a polished aluminium block should be inserted between the
leather and the pad to assist cooling.
5.5 For Transfer of Colour on Dry Rubbing ( Normal Test )
5.5.1 Proceed as in 5.3.1.
5.5.2 Cut each used pad in half along a diameter, and arrange in
sequence on a black card, with half of a clean unused pad beside each, the
cut diameters coinciding. Examine the pads, and decide which is the first
in numerical order of rubs, to show a contrast of appearance with the
unused pads, equivalent to or greater than that given by Grade 4 on the
Grey Scale for assessing staining, or whichever grading is selected as
appropriate. Assess the contrast between the pad which has been given
1 024 revolutions, and the unused pads, using the Grey Scale. If this
contrast is equivalent to or greater than Grade 1, then decide which test
pad is the first in numerical order of rubs to show a contrast of this Grade.
5.5.3 Express the results as: (1) number of revolutions required to cause
a change in colour of the pad equivalent to Grade 4, (2) number of
revolutions required to cause a change in colour of the pad equivalent to
Grade 1 ( if this is 1 024 or less ), (3) contrast grading after 1 024 revolutions
( if this is less marked than Grade 1 ).
5.6 For Transfer of Colour on Dry Rubbing ( Modified Form of
Test for Finishes Which Smear on Rubbing )
5.6.1 Under the standard conditions of test given above in 5.3.1 some
finishes which soften at moderate temperature are found to smear and pick
up small fibres of the felt owing to the rise in temperature. If this occurs,
the fact shall be recorded, and the test procedure modified as follows.
5.6.2 In order to determine the transfer of colour in conditions where
heat build-up does not occur, the procedure of 5.5.1 shall be repeated for
these leathers, but in every test, allowing the finish adequate time to cool
after every N revolutions, N being decided by trial and error so that
smearing or other damage due to heat softening does not occur.
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IS : 6191 - 1971
2. OUTLINE OF METHOD
2.1 The test piece is stored under heat and pressure in contact with filter
paper. The staining of the filter paper is assessed with the standard Grey
Scale.
3. APPARATUS
3.1 Filter Paper — 5 × 5 cm.
3.2 Geometric Staining Scale* — same as 3.2 of LF : 2.
3.3 Smooth Glass Plate — 5 × 5 cm, weighing not more than 50 g.
3.4 Oven
3.5 Weight — 1 kg.
4. TEST PIECE
4.1 Cut a test piece measuring 5 × 4 cm from the sample of leather, to be
tested.
5. PROCEDURE
5.1 Place the filter paper on the appropriate surface of the test piece so that
an area of 5 × 1 cm of the filter paper is not in contact with the test piece
( see Note 1 ). Cover with the glass plate and place the kilogram weight
on the glass plate. Keep in the oven at 60 ± 2°C for four hours. Assess
the staining of the filter paper with the Staining Scale ( see 3.2 ).
NOTE 1 — This procedure ensures that an area of filter paper remains practically
unstained and this considerably facilitates assessment of marking off where this occurs.
NOTE 2 — Filter paper gives a good idea of the marking off properties of a test piece
and is very convenient, but if desired, other materials of interest may be used and
specified.
6. REPORT
6.1 Report the following:
a) Surface of leather tested, and
b) Numerical rating for staining of the filter paper.
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IS : 6191 - 1971
2. OUTLINE OF METHOD
2.1 A piece of finished leather is washed in lauryl sulphate solution of
specified strength. After drying the change in the test-piece is assessed
using the appropriate Grey Scale.
3. APPARATUS
3.1 Glass Drum — 18 cm diameter and 8 cm high, with an opening
fitted with a rubber stopper on one of its flat sides for the addition of liquor
and specimen.
3.2 Rotating Device — This device should be able to rotate the drum
and maintain it at 40 ± 2°C.
3.3 Geometric Grey Scale* — same as 3.1 of LF : 1.
4. REAGENT
4.1 Wash Liquor — Dissolve 5.0 g of sodium lauryl sulphate in about
200 ml hot, distilled water and dilute to one litre.
4.2 Lauryl Sulphate — 85 percent by weight, Min.
5. TEST PIECE
5.1 Cut a 3 × 5 cm test piece from the sample to be tested.
6. PROCEDURE
6.1 Wash the test piece in glass drum under the following conditions:
Float in relation to weight of 1 : 50
the dry composite specimen
Temperature 40 ± 2°C
Duration 30 min
Speed of drum 20 ± 2 rev/min
The milling action on the test piece may be increased by the addition
of glass balls or by appropriate attachment to the stopper of the drum.
6.2 After washing, pour off the liquor. Rinse the specimen in the rotat-
ing drum twice for five minutes in cold, distilled water, float 1 : 50 and
squeeze by hand. Suspend the specimen freely and dry at room
temperature.
6.3 Assess the change in the colour of the leather using the Grey Scale.
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IS : 6191 - 1971
6.3.1 After drying but before assessment lightly stake soft leathers like
gloving.
6.3.2 After drying, but before assessment, brush suede leather in the
direction of the nap with a hair brush ( such as a hat brush ).
NOTE — A very suitable apparatus is that designed for dyeing by Dr Wacker
( glass drum of the dimensions given in 3.1 ). Other machines may be used, provided
they have the same effect as the prescribed apparatus, such as the Launderometer of the
American Association of Textile Chemists and Colourists, or the Washwheel of the
Society of Dyers and Colourists.
7. REPORT
7.1 The report shall comprise of the following:
a) Numerical ratings for the change in colour of the leather;
b) Reference to the present method and any special apparatus ( as
for example, Wacker apparatus ) used;
c) Description of the type of leather;
d) The side of the leather tested; and
e) Details of any deviations from the procedure.
3.2 Rotating Device — Capable of rotating the drum and for maintain*
ing at 40 ± 2°C.
3.3 Geometric Grey Scale* — same as 3.1 of LF : 1.
3.4 Geometric Staining Scale* — same as 3.2 of LF : 2.
3.5 Wool and Cotton Cloth — Unfinished cloth of cotton and wool
3 × 5 cm of plain weave and weighing 125 g/m2.
4. REAGENT
4.1 Lauryl Sulphate — 85 percent by weight, Min.
4.2 Wash Liquor — Dissolve 5.0 g of sodium lauryl sulphate in about
200 ml hot distilled water and dilute to one litre.
5. TEST PIECE
5.1 Cut two pieces of leather, 3 × 5 cm from the leather sample to be
tested.
5.2 Place one piece between two pieces of cotton and the other between
two pieces of wool. Each composite specimen shall be sewn together all
round the edge.
6. PROCEDURE
6.1 Wash both composite specimen in glass drums under the following
conditions:
Float in relation to weight of 1 : 50
the dry specimen
Temperature 40 ± 2°C
Duration 30 min
Speed of drum 20 ± 2 rev/min
The milling action on the composite specimen may be increased by
the edition of glass balls or by appropriate attachment to the stopper of
the drum.
6.2 After washing, pour off the liquor. Rinse the composite specimen in
the rotating glass drum twice for five minutes in cold, distilled water, keep-
ing the float ratio as 1 : 50, and squeeze by hand. Undo the stitching on
both long sides and one short side and dry the composite specimen at room
temperature in such a way that the leather and the accompanying textile
are freely suspended.
6.3 Assess the change in the colour of the leather and the staining of the
accompanying textile using the appropriate Grey Scale ( see 3.3 and 3.4 ).
*Available from Indian Standards Institution, New Delhi.
53
IS : 6191 - 1971
6.3.1 After drying, but before assessment, lightly stake soft leathers, such
as gloving.
6.3.2 After drying, but before assessment, brush suede leather in the
direction of the nap with a hair brush ( such as a hat brush ).
NOTE 1 — A very suitable apparatus is that designed for dyeing by Dr Wacker
( glass drum of the dimensions given in 3.1 ). Other machines may be used, provided
they have the same effect as the prescribed apparatus, for example, the Launderometer
of the American Association of Textile Chemists and Colourists or the Washwheel of the
Society of Dyers and Colourists.
NOTE 2 — If required the test may also be carried out with clothes made of other
fibres such as silk, linen, viscose, acetate polyamide and polyester but should not be
used with leather PVC sheet composites.
7. REPORT
7.1 This shall comprise the following:
a) Numerical ratings for the change in colour of the leather and for
the staining of the cotton and wool, and any other accompanying
textile;
b) Reference to the present method and any special apparatus used;
c) Description of the type of the leather;
d) The side of leather tested; and
e) Details of any deviations of the procedure.
3. APPARATUS
3.1 Fastness Testing Machine — same as in 3.1 of LF : 9.
3.2 Brass Plate — 6.35 mm thick, having a central 25.4 mm diameter
recess, 4.8 mm deep, to receive a felt pad. A convenient size of this plate
is 60.3 × 50.8 mm.
3.3 Felt Pads — Outside diameter 25.4 mm, internal diameter 3.16 mm;
thickness 6.35 mm, medium soft white felt.
3.4 Geometric Grey Scale* — same as 3.1 of LF : 1.
4. TEST PIECE
4.1 Eight separate pieces of leather riot less than 38.0 mm square are used.
Separate small test pieces are used rather than a single larger piece because
diffusion of the solvent may affect the finish at a considerable distance
from the test area.
5. PROCEDURE
5.1 Place the smaller weight on 2the weight platform of the machine. This
gives a total load of 0.72 kgf/cm on the wetted pad including the spindle
weight. Press a dry standard felt pad on the three spikes at a bottom of
the vertical shaft of the testing machine. Place a second standard felt pad
in the hole in the brass plate and position this on the platform of the
machine so that the pad is co-axial with the spindle. ( The brass plate
may conveniently be held in position with bulldog clips. ) Wet the felt
pad evenly with 2.5 ± 0.1 ml of the chosen solvent delivered by a pipette
( see Note 1 ). Immediately after wetting the felt pad, place one test
piece of the leather to be tested on the brass plate with the surface to be
tested uppermost and lower the spindle of the machine so that the dry felt
pad rests on the leather. Allow it to remain in this position for
60 ± 2 seconds. Switch on the motor. After 4 revolutions of the
pad, raise it from the leather and switch off the motor. Repeat this
procedure giving successively 8, 16, 32, 64, 128, 256 and 512 revolutions.
. Between tests remove by blotting any solvent which may remain on the
brass plate. For each test use two new felt pads and a fresh leather test
piece. Hang the leather test pieces to dry in air at room temperature and
arrange them in sequence. Polish the tested areas lightly using a clean
soft doth ( see Note 2 ) and a neutral-coloured soft wax polish, when
necessary to restore the appearance of the leather. Examine the tested
areas and decide which is the first in numerical order of rubs to show, in
its most affected part, contrast of appearance with the untreated leather
equivalent to or greater than that given by Grade 4 on the grey scale in
*Available from Indian Standards Institution, New Delhi.
55
IS : 6191 - 1971
6. REPORT
6.1 Number of revolutions required to cause a contrast of Grade 4 and a
description of the nature of the change; (2) number of revolutions required
to cause a contrast of Grade 1 ( if this is 512 or less ), or contrast grading
after 512 revolutions ( if this is less marked than Grade 1 ) and a descrip-
tion of the nature of the change ( see Note ). Report the nature of the
chosen solvent and specify the surface of the leather which underwent the
test.
NOTE — If desired the discolouration of the felt pads used for each test may be
assessed with the standard grey scale for assessing staining in accordance with LF : 2.
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IS : 6191 - 1971
4. PROCEDURE
4.1 Place a small strip of leather measuring approximately 1 × 4 cm in a
melted paraffin bath at 55°C and keep the paraffin bath for one hour in an
electric oven adjusted to 55°C.
4.2 Transfer the object to a fresh paraffin bath at 55°C for another one
hour or more till the penetration of paraffin into the leather is complete.
4.3 Transfer sufficient melted paraffin into a hollow rectangular mould
formed by two 'L' shaped metal pieces standing on metal or glass base to
cover the bottom.
4.4 With a warm forceps place the object vertically in the hollow
rectangular mould and then fill the hollow mould with melted paraffin.
This shall be added before the surface of the underlying paraffin has
congealed. Orient the object with heated needles to set in the right place
for sectioning.
4.5 When the wax block so formed is partially set, immerse it gently, while
still in the mould, in cold water to ensure rapid cooling.
4.6 When cooled, remove the paraffin block from the mould and trim
down to a suitable size so as to fit the paraffin block holder of microtome.
4.7 Cut sections at a thickness of 50 to 100 microns.
4.8 Remove the paraffin from the sections by placing in xylol for
5 minutes.
4.9 Transfer the sections by section lifter to fresh xylol for another
5 minutes.
4.10 Select one or two of the best sections and transfer them to the centre
of a clean glass slide.
4.11 Drain off excess of xylol, add a drop or two neutral Canada balsam
over the sections and cover them with a clean cover slip. If the sections
are cut from chrome tanned leather use 'Euparol' as mounting medium.
4.12 If the sections are curled up or folded follow the above procedure up
to the step 4.7 then proceed as follows.
4.12.1 Place a small drop of Mayer's albumen on a clean glass slide and
spread it evenly over the surface, with a clean finger. Rub off excess, leav-
ing only a very thin film.
4.12.2 Flood the slide with a few drops of distilled water until the
entire surface bearing the fixative is covered by a thin layer of water.
4.12.3 Take the curled paraffin section with a brush or needle and float
it into the surface of water.
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IS : 6191 - 1971
4.12.4 Warm the slide gently until the section flattens out. Be careful
not to melt the paraffin.
4.12.5 Drain off excess of water and set the slide away to dry. For
quick drying keep the slide in an incubator at 37°C.
4.12.6 Remove the paraffin from the section by placing the slide in xylol
for 10 minutes.
4.12.7 Transfer the slide to absolute alcohol for 5 minutes.
4.12.8 Transfer back to xylol for 5 minutes.
4.12.9 Drain off excess of xylol from the slide and mount with neutral
Canada balsam or Euparol.
LM : 2 FREEZING METHOD
1. SCOPE
1.1 This method is suitable for the preparation of microscopical slides
from green, wet-salted, dry-salted and dried hides and skins, pelts and wet
tanned leathers.
2. APPARATUS
2.1 Cover Slips
2.2 Forceps
2.3 Freezing Microtome
2.4 Glass Slides
2.5 Needles
2.6 Section Lifter
2.7 Petri Dishes
3. REAGENTS
3.1 Formaldehyde Solution — 10 percent ( w/v ).
3.2 Gum Mixture — Dissolve 5 g of gum arabic, 1 g of boric acid, 1 g of
sucrose in 100 ml of distilled water and filter through cotton plug.
3.3 Glycerin Jelly — Warm 650 ml of distilled water in a 2 litre beaker
to about 40 to 50°C. Then add 100 g gelatin on the surface of the water
a little at a time, stirring in each lot with a glass rod; then add and stir in
100 g of glycerin. Add a bit thymol for preservation.
4. PROCEDURE
4.1 Cut a small piece measuring approximately 5 × 10 mm from formalin
( see 3.1 ) fixed hide or skin. Wash the object in running tap water for
about 20 minutes. Put a little gum mixture on the freezing disk of the
microtome and place the object in it in such a way that longitudinal sections
59
IS : 6191 - 1971
may be cut. Surround the object with gum mixture and open the valve
very slowly. As soon as the gum mixture is frozen, continue to add more
until the object is completely covered and frozen. Cut section at
40 micron and collect the sections in distilled water ( water should be
changed to dissolve out the gum ).
4.2 Take a small piece measuring about 25 mm square and leave it in
running tap water till soaked back. Keep the soaked piece in 10 percent
formaldehyde solution for fixing for 24 to 72 h depending on the thickness
of the sample.
LM : 3 STAINING TECHNIQUE
1. SCOPE
1.1 This method prescribes the solutions required and describes the
technique employed in staining the frozen section described in LM : 2 for
fat, bacteria and mould and paraffin section for calcium and iron.
2. STAINING FOR FAT
2.0 Scope — All samples should be cut in freezing microtone including
picking band and belting leathers.
2.1 Reagents
2.1.1 Staining Solution — saturated solution of Sudan IV (Scharlach R)
in 70 percent alcohol.
2.1.2 Ethyl Alcohol — 50 and 70 percent solutions.
2.2 Procedure — Pass the frozen sections through 50 percent and 70 per-
cent alcohol keeping 2 to 3 minutes in each. Transfer to the saturated
solution of Sudan IV in 70 percent alcohol for 15 to 20 minutes. Wash in
50 percent alcohol for 2 to 3 minutes. Transfer to distilled water. Mount
in glycerin jelly.
2.3 Observation — fat glands and fat droplets stain red.
3. STAINING FOR BACTERIA AND MOULD
3.1 Reagents
3.1.1 Ethyl Alcohol — 50 percent, 70 percent and absolute alcohol.
3.1.2 Staining Solution — methylene blue; aqueous 0.5 percent solution.
3.2 Procedure — Transfer the frozen section to 0.5 percent methylene
blue solution for 10 to 20 minutes. Wash in distilled water. Dehydrate
by passing through 50 percent, 70 percent and absolute alcohol, keeping
2 to 3 minutes in each. Clear in xylol. Mount in neutral Canada balsam.
Chrome and vegetable tanned sections are immersed in 1 percent potassium
permanganate for 15 to 30 minutes, transferred to 2 percent sodium
metabisulphite until sections are colourless. Wash in distilled water;
60
IS : 6191 - 1971
62