Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
to the public, particularly disadvantaged communities and those engaged in the pursuit of
education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.
1 +, 1 +
01 ' 5
Jawaharlal Nehru
! $ ' +-
Satyanarayan Gangaram Pitroda
! > 0 B
BharthariNtiatakam
Indian Standard
METHODS OF SAMPLING AND TEST
FOR OILS AND FATS
PART 1 SAMPLING, PHYSICAL AND CHEMICAL TESTS
(Revised)
Fourteenth Reprint JULY 2007
(Incorporating Amendment Nos. 1 to 4 and Including Amendment No.5)
Copyright 1976
October 1964
CONTENTS
PAOE
o.
1.
SCOPE
2.
TalUllNOLOOY
3.
SAlfPUNO
4.
QuAUI'Y OP Ru.OI.NTI
18
5.
18
6.
28'
7.
29
P.
DaftlUllNATlON
9.
"
10.
35
11.
39
0.
3.
UNIAPONmABLE MATl'ER
42
13.
45
DaTZUONAnON OF CoLOuR
VALUE (WIJI)
47
50
DETERMlNAnON
IODINE
0"
AaTYL
V ALUI
VALva
17.
DaftllMlNAnON o.
ALLYL
isttnuOCYANATE
AND
HYDROXYl.
52
56
18.
57
19.
62
21.
DETERMINATION
or
PEROXIDE VALUE
63
Indian Standard
METHODS OF SAMPLING AND TEST FOR
OILS AND FATS
PART I SAMPLING, PHYSICAL AND CHEMICAL TESTS
( Revised)
Oils and Fats Sectional Committee. CAFDC 5
a"
Rt/w.SM/UtI
CA.i,...
Da J. S.
BADAMI
M"'*'J
SR.' V. A. 'A.ntH (
Dr J. S. Badami)
AI",,..,, to
SKa. S. K. Bosl.
SKa' V. V. DAN' ( Allmllllt )
SHU
C. R.
OM
SHa. N. DUlltAcHAa
Da B. G. GUNDZ ( Alln"al, )
K. C. Guun
n.
or
511&. K. P.JAIN
SHa. F.O. T.
, ... R. K.
MENEZES (
MALIK
StUu K. L. CHATTRJE
Da 8. D. NARANG
Al""ud, )
Directorate or Marketinl at Inspection (l\iiniltry
Food It Asricuhure)
( Alit,,,,,,)
na M. S. PATEL
SMa. H. P. R. RAJA
SHK. CHAIANDAS
(Alt"",." )
Da H. G. R.
or
V. MAR1WALA
ofTtchnicallkvelopment
REDDY
S...I R. C. Mila"
Extra AIIistanl Director ( Chcm ), 151
.,.,."
2)
e-r..r
RI/Jr,ulllinl
HiDdUitan Lever Ltd, Bombay
Da G. 8. HAnIANGDI
11..-,
c...r
Da s. M. PATaL
MtmMrJ
SDI N. DIIIXACliAil
Da B. G. GUND& ( AI,.",.16)
DaJ.G.KANa
.... 1l.K.M.wx
of C,.",.1Il lim..
loU. Ultiwrsil.1 ofBttmbll.1, BomIJtI,1 )
Directorate of Marketing &. Inlpection (Miniltry
of Food at Agriculture)
( AllmJlJII )
Ministry or Defence- ( R" D)
In personal capacity ( Dt/NI"m",'
8DJ X. L. CHATrUJI.&
.... I. D. SINOR
.... R.. P. VUIIA( .4"",.",. )
Da A. R.
SUIQ)AJlA&AJAM
Health)
(Page 10. clause 11.0) - Add the following new matter at the end
of the clause:
'Method A shall be used as a referee method whereas Method B may be
used for routine analysis.'
19.1 OutliDe of the Method - Oils, fats and other interfering substances
are removed from the colours by solvent partition technique using dimethyl
forrnamide and hexane (3: 1 ), followed by alumina adsorption. The
colours are detected by reversed phase paper chromatography.
19.2 Apparatu8
19.3 Reagents
19.3.1 Hexane
19.3.2 Dimethyl Formamide
19.3.3 Sodium Chloride Solution - saturated.
19.3.4 Alumina Neutral, Brockmann, Activity 1 ,for Example, Made by National
Chemical Laboratory, Punt or of Equioalm: Quality - activated at 100C for
4 hours.
19.3.5
19.3.6
19.3.7
19.3.8
19.3.9
Diethyl Ether
Ethyl Alcohol
Ammonium Hydroxide Solution
Methanol
Petroleum Ether - B. P. 40 to 60C.
Prepared by
soaking the paper in 5 percent liquid paraffin in petroleum ether and subsequent drying in air.
19.3.12 Oil Soluble Colours - Butter yellow, Cres orange GN, Sudan IV,
Gress Yellow GRN type, etc.
if necessary.
this treatment any minute curcumin and turmeric will come to the ether
layer.
19.4.3 Separation of Natural Colours from Synthetic Oil Soluble Colours Clamp the chromatographic tube and pour 40 ml of hexane with the nongreasy stopcock in closed position. Place a cotton plug ( if no fritted glass
is fixed in the tube) firmly at the bottom of the tube. Pour 40 ml of
hexane followed by anhydrous sodium sulphate to form a 2 to 3 ern layer.
Now open the stopcock to give a trickle of solvent and tap the tube. Pour
alumina sufficient to give a column of 10 em length into the solvent with
constant tapping. This will give a channel-free column. It is important
that the top of the alumina is always under the solvent. When the solvent
layer reaches about 1 em above the alumina, pour the hexane extract of
colours-carefully into the tube. Collect the eluent in a beaker. Continue
the elution with four batches of 10 ml hexane. Concentrate the eluate
containing oil soluble synthetic colours. After elution with hexane pass
40 ml of another eluting solvent, namely, petroleum ether: acetone ( 1 : 1 )
for complete elution.
19.4.4 Detection of
Oil Soluble Colours - Cut a reversed phase
chromatography paper to a size of 20 X 20 em, Then draw a straight line
by a lead pencil on the paper leaving away 3 ern from the bottom. Spot
the concentrated extract (say 10 ""lor more according to the colour
present on the solution) and also some known oil soluble colours on the
line drawn on the reversed phase chromatography paper leaving 1 em
distance from each other. Then make the paper to a cylindrical shape,
staple it and dip in anyone of the solvents ( see 19.3.19 and 19.3.20 ) for
ascending chromatography. Run for 10 em, The development in the solvent
given under 19.3.19 takes 45 minutes and that in solvent prescribed
under 19.3.20 takes one hour. Take out the paper, dry in air and detect
the colour by comparing with the known colour in respect of shade and
Rfvalues.
19.4.5 Detection ofNatural Colou,s - Elute the natural colours absorbed on
the column by the solvent methanol : ammonium hydroxide (9: 1 ) and
then examine for natural colours. If colour of the column changes to red.
violet after passing the above mentioned solvent, it confirms the presence
of curcumin or turmeric.
portion add boric acid solution to make the solution acidic. If red colour
appears, turmeric is present and if pink colour appears it indicates the
presence of curcumin, Sometimes turmeric and curcumin are not eluted
if present in small amount. Notice the change of colour of the column
for their detection.
(CAFDC 5)
Indian Standard
METHODS OF SAMPLING AND TEST FOR
OILS AND FATS
PART I SAMPLING, PHYSICAL AND CHEMICAL TESTS
( Revised)
o.
FORE WORD
SAMPUNO
Standards Institution.
or
5
FATI AND
FATTY
Ons,
British
ANALYm o. OIU
AND
FAn.
ilritish
British Standards
Methods of S&lY\fling
and Testing Vegetable Oils and Fats under Agmark ( Matketing
Series No. 78). New Delhi. Manager of Publications, 1952.
Methods of Sampling
and Testing Butter-Fat (Ghee) and Butter under Agmark
( Marketing Seria No. 81). New Delhi. Manager
Publications, 1953.
or
1. SCOPE
1.1 This standard lays down the methods of sampling and test for individual oils) rats and fatty materials. It contains definitions of terms \lied
in trade arid industry and prescribes the methods for determining moisture,
.insoluble impurities, acid value and free fatty acids, unsaponifiable matter,
melting point, refractive index.sspecific
titre of mixed fatty acids,
colour, iodine value (Wijs), saponification value, acetyl value and
hydroxyl value, allyl isothiocyanate content, Reichert-Meissl value and
2.TEIIMlNOLOGY
2.0 Fer the purpose uf this standard, the following definitions shan apply.
ODe
2.2.1 The acidity of the oil or fat indicated by its acid value is frequently
expressed as free fatty acids present in the sample.
2.3 Hydrosyl Val.e - The number of milligrams ofJX?tassium hydroxide
required to neutralize the acetic acid capable of combining by acetyl.tiOD
with one gram of the oil or fat ( s" also 201 ).
2.3.1 Hydroxyl value is equivalent to the hydroxyl content of the
material based on the weight of the unacetylated fat.
2.5.1 The iodine value of the oil or rat gives an indication of the dqree
of unsaturation of the constituent fatty ,iycerides. It is customary to pve
the method employed for its determination, Wijs method is apphcable to
all normal oils and fats not containing conjugated systems.
2.6 Meldal Polat - The temperature at which the oil or rat
or
becomes
fluid to slip or run u determined by the open..tube
capillary-slip method. In the case
the closed-tube complete-fusion
or
2.12.2 Specific Gravity of a Fat - The ratio of the weight in air of given
volume of the fat at 95C to the weight in air of an equal volume of
water at 30C.
2.13 Titre - The hi,hest temperature attained under standard conditions,
during the solidification of the mixed fatty acids obtained from the oil or
fat.
.
s. SAMPLING
3.0 Geaem- It is very difficult to lay down detailed directions for
sampling oils and rats that will encompass all conditions and circumstances
which may confront the individual charged with the responsibility of
taking the sample. There are many instances in which the experience and
judgement of the individual should prevail. There are, however, certain
general rules relating to the drawing. preparation, storage and handling of
samples which should always govern if the sample is to be representative.
These are described under 3.1 to 3.8.
pling instruments may be cleaned with hot soapy water or other detergent,
care being taken to wash away the last traces with scalding hot water. If
a source of steam is available, the instruments may receive a final cleansing
in a jet of steam and it is recommended that this procedure be carried out
when edible" oils are sampled and where the taste is likely to be of primary
importance.
3.13 Samples shall not be taken in an exposed place. The samples, the
material being sampled, the sampling instruments and containers for
samples shall be protected from adventitious contamination. The tcst
samples shall be placed in suitable clean and dry containers.
3.1.4 Samples shall be stored in such a manner that they are protected
from light, temperature fluctuations and other abnormal conditions.
3.1.5 Sample containers shall be so filled that the air space above the
liquid level shall be 5, to 10 percent of the capacJty of the sample
containers.
Fro. 1
SAMPLING BOTTLE OR
CAN
3.2.2.1 CIDsld-type stJmpling tub" undividtd - It consists of two concentric metallic tubes closely fitted into each other throughout their
entire length, so that one tube may be rotated within the other. Longitudinal openings of about one-third the circumference are cut in both
tubes. In one position the openings in the two tubes coincide; the sampling tube is open when in this position and adJ!lits the material. By
turning the inner tube through an angle of 180, it becomes a sealed container. The inner tube may have a diameter of 2Q to 40 mm and is
undivided along its length to serve as a single container ( s" Fig. 2).
The two concentric tubes are provided with ports at their bottom
ends, 10 placed that it becomes possible to drain the material contained in
the instrument through them, when the longitudinal openings coincide.
The
of the instrument should be such as to enable it to reach
the bottom ef the container being sampled.
The instrument is inserted closed. the material is admitted by opening
it, and finally, it is closed and withdrawn.
10
IS I 548 ( Part I
CLOSED
OPEN
PORTS
OPEN
CLOSED
t:J::.\
10TTOM VIE WS
Flo.
UNDIVIDED
:0
ENLARGED
SECTION XX
ENLARGED
SECTION VY
1 1
I I
I I
1 I
I I
'4
I I
I
II'
I
I I
I I
".
I
...
I
I
I I
TUBE
St-IJTTER
IS.
5.
(Part )-1'"
3.2.3 Sampling SeoO/Js - These instruments are of the open type and
are suitable for taking samples of naturally occurring vegetable fats or
6TO 12mmDIA
...o
..,
20 TO 40 mm OIA
, TO 40mm t'lt'
FlO.
of
OPEN-Tvp.. SAMPLING
IS I M8 (Part I )-196t
hydrogenated vegetable oils. They are of metal, of leItli-circular 01'
C-shaped cross-section, and will bore out a core of the sample throuah
the material being sampled (s Fig. 5A and 5B).
o
I
'----I' "l---'
FlO.
5A
SAMPLINO ScooP
FlO.
5B
SAMPLINO ScooP
14
15
IS I M8 ( Part I)-19M
a) Liquid oils
16
T"""s
17
samples of each of the separate qualities ( st, 3.4.2.2) for compliance with
the requirements of the individual specification, or he may prepare, for
the purpose of such examination and at any stage of the progress of the
examination, a composite sample representing the whole of the consignment, by mixing the test samples.
4. Q,VALITY OF REAGENTS
4.1 Unless otherwise specified, pure chemicals and distilled water [,.
IS: 1070-1960 Specification for Water, Distilled QJ.1ality ( RAllisM)] I&all
be employed in tests.
r.on - ' Pure chemical. mall mean cbemicala that do not contain impuriti. which
afl't.ct the resul tI
or
18
or
or
5.1.3 C"bltllion
100
--w
III
&IB
where
w
5.2.1 Apparalru
5.2.1.1 Glass b,dk" -
5.2.3 Calculation
100 w
== -w-
where
Nominal Dia
of lArge End
of Ground Zone
N aminal Dia
of Small End of
Ground Zone
mm
mrn
18-8
Nominal l,tngth of
Ground Zone
Axially
mm
26
11. Me ( Part I
CONDENSER
OtSTIl\,A'TtON
FLASK
FlO.
22
25
23 TO 25 00
WAll 1 TO 15
THICK
250
16 TO 17 00
WAll 0'7 TO 1 .../
THICK - - -
2S
B LENGTH
All climeaaioD. ill miUimetra.
Flo. 6A
CoNDSNI.a
The fthoulder of the upper chamber of the receiver immediately below the conical joint shan be finished square, as shown in
Fig. 6B and 60. The graduated portion of the receiver shall be
cylindrical throughout its length. The bottom of the graduated
tube of the 2-ml receiver shall be sealed, the end of the tube
being approximately hemispherical in shape. The graduated
scales on the receivers shall be numbered and subdivided as shown
in Fig. 6B and 60. The graduation marks shall be fine cleanly
in planes at
etched permanent lines of uniform thickness
right angles to the axis of the tube. The graduation marks shall
be confined to the cylindrical portion of the tube and there shall be
23
IS I M8 ( Part I )-1964
TAILB I MANDATORY DDIENIIONI AND TOLIDlANCE8 POR RECBIVEIl
(Cl." 5.S.I(c)]
St. No.
IQ-ml
(2)
(4)
0'1
(I)
il)
Scale lenllh. mm
iii)
.topcock,ml/min
9S! 10
70
100. . .- - -
1104
90
AU dimCDlioaa ia miWmetra.
Flo. GC 10ml
26
RacBIVIUl
5.3.2 ReQgents
5.3.2.1
dich,omtJt,-sulphuric iJ&id cleaning solution
5.3.2.2 Xyl,ne or loluine - Saturate the xylene or toluene by shaking
with a small quantity of water t and distil. Use the distillate for the determination of moisture.
5.3.3 Procell"rl - Clean the entire apparatus with potassium dichromate..
sulphuric acid cleaning solution to minimize the adherence of water
droplets to the sides of the condenser and the receiver. Rinse thoroughly
with water and dry completely before using. The quantity of material
taken for the test is determined by the amount of moisture present (wJw),
as indicated below:
(};lantily of MiJU,iGI
)
200 g
100 g
Moisture Range
27
5.3.4 Calculatioll
M"J.olsture
'
ht
eontent, percent b y weig
100 VD
-= -W-
where
V ac volume in ml of water,
D =- specific gravity of water at. the temperature at which the
W -=
6.0 Geaeral- The material is dissolved in hot kerosine and filtered. The
residue is washed thoroughly with petroleum ether dried at 100
and cooled in a desiccator till constant in weight,
200
6.1 Apparata.
6.1.1 Gooch Cruei6lt -. prepared with a pad of acid-washed asbestos,
aboul2 mm thick. \Vash the pad with water alcohol and ether. Dry to
1.2
aeacea ts
28
1.3 Proc. . . . - Use the whole of the heated oil or rat lell over after the
determidation of moisture and volatile matter described under 5.1 or 5.2.
AllmIlJli",l:1, use a sample prepared in the same manner. Add 50 ml
kerosine to this quantity of the oil or fat and heat on a water-bath to
dissolve it. Filter through the prepared Gooch crucible with the aid of
vacuum. Wash the container and the crucible with five IO-ml portions of
hot kerosine allowing each portion tn drain before adding the next. \Vash
the crucible thoroughly with petroleum ether to remove all the kerosine.
Dry the crucible and contents to constant weight at 100 2O, cool to
room temperature in a desiccator, and weigh.
or
6.4 CalcaladoD
impurities, percent
by weight
=-
100 w
-w-
where
w = gain in weight in g of Gooch crucible, and
IV
== weight
7.1 Rea.eat.
7.1.1 Ethyl Alcolaol- ninety-five f!ercent ( by volume ), or rectified spirit
[conforming to IS: 323.. 1959 Specification for Rectified Spirit ( Revised) ]
neutral to phenolphthalein indicator.
7.1.2 Phtnol/Jlat1ull,in Indicator Solution - Dissolve one gram of phenolphthalein in 100 ml of ethyl alcohol.
Non - \Vhrn tratinl oill or fatl which give dark coloured loap solution, the
oblervation of the end point of the titration may be f.cilitated rither <a> by Ulinc
or alkali blue 68 in place of phenolphthalein, or (b) by addin.
one millilitre of a 0'1 percent ( wlu ) solution of I:lcthylene blue in water to each 100 mJ
of phenolphthalein indicator solution before the titration.
0'
7.2 Procedare - Mix the oil or melted fat thoroughly before weighing.
\\'eigh accurately a suitable quantity of the cooled oil or
29
fat in
7.3 Calculatioll
.
ACId value
==
56'1
VN
where
v ==
7.3.1 Free Fatty Acids - The acidity is frequently expressed as the percen- '
tage of free fatty acids present in the sample. The percentage of free fatty
acids in most of the oils and fats is calculated on the basis of oleic acid;
although in coconut oil and palm kernel oil it is often calculated in terms
of lauric acid, in castor oil in terms of ricinoleic acid, and in palm oil in
terms of palmitic acid. The calculations in terms of different fatty acids
are as follows:
a) Free fat ty acids, in terms of oleic acid,
28'2 VN
percent by weight
W
v == volume
used,
8.1 Apparata.
8.1.1 F1Qt-Bottomed or Coni,,,' Fla.sk - 250 to 300 ml capacity. An ordinary round, flat-bottomed flask, fitted with a long glass tube which acts as
a condenser, may also be used.
8.2 ReageDt.
8.2.1 A/roholic Pol4Ssium Hyd,ox;u Solution - Dissolve 70 to 80 g of potassium hydroxide in an equal quantity of distilled water, and add sufficient
aldehyde-free ethyl alcohol (95 percent by volume) or aldehyde-free
rectified spirit [conforming to IS: 323-1959 Specification for Rectified
Spirit ( Revised) ], prepared as described under G-3.4 of IS : 323.1959. to
make up to 1 000 ml, Allow to stand overnight, decant the clear liquid
and keep in a bottle closed tightly with a cork or rubber stopper,
8.2.2 Ethyl Alcohol- ninety-five percent ( by volume). or rectified spirit
[ conforming to IS : 3231959 Specification for Rectified Spirit ( Revised) ].
8.2.3 Phenolphthalei" Indicator Solrltion -- Dissolve one gram of phenolphthalein In 100 ml of ethyl alcohol.
8.2.4 Petroleum Etla" - conforming to solvent Grade 60/80 of *IS : 17451961 Specification for Petroleum Hydrocarbon Solvents.
8.2.5 Aqutous Alcohol- containing 10 percent (by volume) or ethyl
alcohol [conforming to -IS: 321-1952 Specification for Ethyl Alcohol
( Absolute Alcohol) ].
8.2.6 St"ndard Sodium HJflroM S,I",ioJl- approximately 002 N.
8.2.7 Aceton, - free from evaporation residue (su 15: J701950 Specification for Acetone ).
8.3 Proceclare
8.3.1 \\'eigh accurately about 5. of the well-mixed sample into the fluk.
Add 50 ml of alcoholic potassium hydroxide solution. Boil
but
steadily under a reftux condenser for one hour or until the saponification is
Since revised.
31
8.4 Calcaladoa
8.f.l Weight in g or the fatty acids in
the extract ( as oleic acid) -= B
0282 VN
where
1,- B)
( '" 1.3.2),
(s', 2.& ).
9.0.1 The melting point is determined by taking the solid fat inside a
small capillary tube and two methods are prescribed for the purpose. Both
of these are applicable to all types of normal animal and vegetable fats and
the method used shall be specified while stating the results.
heating
arrangement.
Thiele
or
33
9.2.1 App",atllJ
9.2.1.1 Melting /Join' tu6s - thin-walled, uniformly bored capillary
glass tubes open at both ends and with the following dimensions:
a) Length, 50 to 60 mm;
b) Inside diameter, 0-8 to 11 mm; and
c) Outside diameter, 12 to 1-5 mm.
s""" -
1.2.2 Proe,tlur, - Melt the sample and filter it through a filter paper
to remove any impurities and the lut traces of moisture. Make sure that
the sample is absolutely dry. Mix the sample thoroughly. Insert a clean
melting point tube into the molten product so that a column of the material about 10 mm long is forced into the tube. Cautiously fuse one end of
the tube (where the II'mple is located ) in a small flame, taking care not
to bum the fat_ Place the tube in beaker and while the fat is still in the
liqui41 state. transfer to reCrisera tor and hold at 4 'to 10C overnight
(about 16 houri) _ Remove the tube from the refrigerator, and attach
with a rubber band or by any other luitable means to the thermometer 10
that the lower end of the melting point tube is even with the bottom of the
bulb of the thermometer. Suspend the thermometer in a large test-tube
containing water and Immerse it in the 6OO-ml beaker which is about half
full of water. The bottom of the thermometer is immersed in the water
about 30 mm below the surface. Adjust the starting bath temperature
from 8 to lOC below the melting point of the sample at the belinning of
the test. Agitate the water in the large test-tube as well as in the beaker
with a small stream of air or by other means. and apply heat so u to
increase the bath temperature at the rate of about O-SC per minute. As
35
'JD
1-4220
4-7
1
2
3
4
5
6
7
8
9
.'8
8
9
1-4260
I
9-5
9'6
9-8
g'g
2
3
10-0
lOti
103
10'4
6
7
10'5
'WID
0-0
0-1
0-2
2
3
4
5
5'0
5-1
5'2
5-.j.
5'5
S"6
5'7
5-9
6-0
6-1
6'2
6'46'5
6-6
6'
6-8
6'9
2-4
2-5
7
8
9
1-424 0
2-6
0-4
0-5
0-6
0'"
o-s
10
I-I
1-2
1-4
1-5
1-6
1-7
i-s
2'0
2'1
2-2
2-7
28
3-0
3.1
3-2
3-3
5'5
3'1)
S-7
S-8
4'0
4'1
4-2
4'3
4'5
4-6
5
6
7
8
9
7-0
7'1
7-2
7--1
7'5
(0-6
10-1
10'9
11-0
11-1
11'3
11-4
I)-S
11-6
11-8
11'9
12'0
12-2
1-4280
12'3
:t
7'6
12-4
4
5
6
1-7
7'9
2
3
12'5
12'9
1'4230
1
8'0
8-1
8'2
8
9
1'4-27 0
I
2
3
4-
12-7
12-8
"lJD
8
9
1-4300
1
2
3
4
5
6
7
8
9
1'1310
1
2
3
4
5
6
7
8
9
1-4320
I
2
3
14-4
14-5
14-6
14-7
If-9
15-0
15'1
IS"!
15"4
15-5
15'6
15'S
15'9
16-0
16'2
16-3
16'4
16-6
16.7
16'8
17-0
17'1
17-2
17'4
17-5
17-6
178
17-9
18'0
1'4250
8-5
8-6
2
3
8'7
5
6
7
8
9
1'4290
13-6
4
5
6
7
8
8'9
13-7
2
3
4
5
15-8
14-0
1'4!50
18-9
14-1
14-2
2
S
19-1
7
8
9
45
6
7
8...
g-O
9'1
9'2
9-4
13'0
1"2
13'3
13'5
18'2
'JD
45
6
7
8
9
"i34 0
I
2
3
4
5
6
1
8
9
)'''350
I
2
.
3
7
8
9
14360
I
2
!
IS-S
18'4
.5
6
18-5
18'7
IS-8
19-2
7
8
9
1-4370
I
1ID
19-5
19-5
19-6
19'7
19-8
20'0
20-1
2
:J
4S
20'5
6
7
8
9
1tlf380
I
20'6
20'8
20'3
20-.
20'9
21-1
21'2
5
6
21-3
21'.
8
9
1'4390
I
21'6
21-7
21'8
22'0
22-1
222
22'40
22-5
22'6
2
:4
4-
5
6
22-7
22-9
23-0
23'2
23-5
23'
8
9
1'4400
I
23-5
23-7
23'8
5
6
7
8
2S-9
24-1
24-2
,
2
( CMIirnIM)
aurrao
TAIU.& 2 CONVBBIION OP
RlDACTOaa:n& aBADINGI
( B ) TO aBl'L\CTIVB INDica ( 1) D ) - GMI4
1ID
1JD
24'S
1441,0
so8
8
9
J"4-f6 0
375
246
24-7
24'8
250
25-1
252
25-4
25'5
256
25'8
259
26-1
262
265
26-5
26'6
26-7
26-9
270
27"1
275
274
27'S
277
27-8
27-9
28'1
28'2
283
28"5
286
287
289
290
29'2
295
29-4
296
29-7
299
90"0
SO-I
SO-S
SO,t
306
so 7
1
2
S
4
5
6
7
8
9
1442 0
2
3
45
30"9
31'0
31:
2
S
32'2
:42'3
325
32'6
8
9
1-4470
I
328
32'9
55'0
33'2
8
9
333
39'S
33'6
33"
33'9
34'0
34'2
34'S
14430
1
2
:4
45
6
7
8
9
t4+t 0
2
5
.5
6
7
8
9
14450
I
2
4-
6
7
31'4
31'5
51-6
31'8
31-9
32'1
3i'.
34'6
Sf,
54'9
5S'0
35-1
35'3
355
35'6
35'7
35-8
!6'O
36'1
36'3
36'"
36'5
367
36'8
37'0
971
37'2
37-4
..
5
6
7
2
3
45
6
7
8
9
14480
I
2
3
f
5
6
7
8
9
1-4490
I
2
3
4
5
6
7
8
9
1-4500
I
2
3
4
5
37-7
7
8
9
37-8
37'9
381
38'2
38'3
385
386
387
38'9
390
39'2
sg.!
3g.,
39"6
t-flj! 0
1
2
3
5
6
7
8
9
14520
I
397
39'9
..5
40-0
40-1
40'3
40'4
40'6
40"
41'0
fJ')
41-S
41-"
6
7
8
9
1-4530
I
2
S
..5
41'S
41'7
6
7
8
9
418
42'0
42-1
42'5
424
425
42'7
42'S
43'0
431
43'3
43-4
43'6
437
4:t9
44'0
44'2
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1-4540
I
2
3
4
5
6
I)
9
l'45S 0
1
2
3
44'
44".
44-6
...7
44-9
4S-0
45'2
45'3
4S-S
45-6
45'7
45'9
46"0
462
40-3
1JD
1ID
5
6
.51-4
"J-6
51-7
51"9
51'
2
S
f
..
7
8
9
1'456 0
I
2
3
52-0
52'2
52'3
52
5353-I
53'3
46-6
46'7
469
47'0
2
3
54-0
5
6
7
8
9
I
2
3
54-5
546
M8
55-0
55-I
55'S
55-4
55-6
557
.562
.'"2
47'3
47'5
47-6
477
47"9
fBO
482
1'.580
48-5
.-5
48-3
48'6
48'8
48'9
49'1
49'2
49'4
49'5
49'7
49'S
SO-O
50'1
50-2
SO'.
SO'S
50'7
SO'8
51-0
51'1
7
8
9
1"4590
I
2
.
3
5
6
7
8
9
14600
I
9
"4610
525
5
6
7
8
9
1'4570
46.
6
7
8
53..
53-6
S3'7
559
54-2
54S
55-9
56-0
56'S
56"5
566
568
56-9
571
57"
57-4
576
57-7
57"9
58'0
58-2
58'3
58'S
1
2
S
4
6
7
8
9
1'4620
1
2
S
4
5
6
7
8
9
1'46' 0
I
2
3
f
9
1"4640
,
1
2
4
5
6
7
8
9
(CMIiuItl )
37
B
58"6
58'8
58-9
59-I
"D
'In
1'4650
1
66"2
9
1'4700
I
2
3
74'0
'.-1
66-4
66-5
59'2
3
4
66-8
59'4
59-S
5
6
59-7
59-&
6&0
60'2
603
60-5
60-6
60-8
6&9
61-1
61-2
61-4
61-5
61-7
61'S
62-0
7
8
9
1'466 0
..53
6
7
8
9
1'4670
66"7
67'0
6;'2
67'3
67-5
67'7
67'8
68'0
68'1
68'3
68-4
68-6
68-7
68'9
69'1
69'2
69'"
69
62-2
I
2
3
62-5
62-6
62-8
62-9
63-1
5
6
7
8
9
70'2
1'468 0
I
2
3
71"0
71'1
71'3
&2-4
63-2
63-4
63-S
63-7
63-8
64'0
64-2
64-3
64-5
64"
64-8
6.5-0
6.5-1
6S-3
65-4
65'6
65-7
65-9
66-1
-to
7
8
9
1-469 0
I
0S
69'7
69-9
70-0
70'3
70'S
'0-7
10-8
71-.
716
71'S
7J09
72-1
722
72.
72-5
72-7
72-9
7S0
732
7S'!
73
73-7
73'S
5
6
0S
..
5
8
9
1-471 0
J
2
3
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6
7
8
9
)....7 20
1
9
1-4730
J
2
82-5
83'1
83'2
83'.
75'3
7S-S
756
75-8
760
76'1
16-3
76-3
76'7
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6
8
9
1-.760
1
2
3
4
5
76'8
77-0
6
7
8
77-2
77'3
77'5
786
78-7
78'9
79-1
79'2
79-4
3
4
G
7
8
9
1-.780
I
2
S
f
8&3
5
6
8&8
81'0
81'2
81-3
81
81-7
81-9
82-0
82-2
83-6
83-S
83'9
84')
84-3
84-5
84-6
(Ha
85'0
85-2
85"
8SoS
85-'
85'9
86-0
1'4-770 86-2
1 86'..
2 86'6
7 8&5
8 8&6
.
.5
91"1
74'5
80-1
2
S
7
8
9
1'4800
14'6
7.'8
75'0
7S'1
9
1-47.0
J
82"4
82-7
82-9
"lJ D
1-475 0
79-6
790S
SO-O
8
9
7'-'
77-7
2. 77'9
3 781
4 782
5 78.
6
7
1J D
8
9
1'4790
I
2
3
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6
38
86-7
869
87-1
87-3
87-5
876
87-8
88-0
882
88-'
88-.5
88-'
889
89-1
89-2
1
2
3
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6
7
8
9
I-fBI 0
I
a
4
5
6
7
8
9
1'4820
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6
7
8
9
1-483 0
2
3
..
5
6
89'4
&6
89-8
90-0
90-2
90-3
90-5
go-7
90-9
9
1-'" G
J
2
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:I
91'2
91"491'6
91-&
92-0
92'1
92'S
92'5
92'7
929
.930
93-2
93'4
93-6
93'8
94'0
M-I
94'3
94-5
94-7
94-8
95'0
952
95f
95-6
95-8
960
96'1
963
960S
967
969
970
97-2
97-4
97'6.
97-8
98'0
98-1
98-3
98'.5
98-7
989
99-1
99'2
99'f
99-6
99-8
100-0
'ID
,
6
1-4851
i
45
7
8
9
1-4860
1
2
..s
3
7
8
9
104CJ:-O
I
2
3
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5
6
7
B
9
1
1
3
4oS
9
1-4890
..
I
1-489 5
TOC/ToC
D' + 0000 64 ( T' - T)
a ) S peeifi c gravity at
- W, + 0.000 23 ( T' _ T)
where
D' = density of oil fat at T'OCj
T" - the temperature at which the densities D' and W' were
determined;
T == the standard temperature. 3QC; and
W' =- density of water at T'oC.
39
+ 0000 41 ( T'
- T)
where
11.3.1 Appartllus
11.3.1.1 Specifie ,ravil.J hollu or pyknometer - with well-fitting ground
glass joints, To calibrate, clean and dry the bottle or pyknometer
thoroughly, weigh and then fill with recently boiled and cooled water at
about 250 after removing the cap of the side arm. Fill to overflowing
by holding the bottle or pyknometer on its side in such a manner as to
prevent the entrapment of air bubbles. Insert the stopper and immerse
In a water-bath at the desired test temperature O2C_ Keep the
entire bulb completely covered with water and hold at that temperature
for 30 minutes. Carefully remove any water which has exuded from the
capillary opening. Remove from the bath, wipe completely dry, replace
the cap, cool to room temperature and weigh, Calculate the weight of
water. This is a constant for the bottle or pyknometer, but should be
checked periodically, A specific gravity bottle of about 50 ml capaeity
and of either of the two shapes as shown in Fig. 7 is recommended.
11.3.1.2 Walerbalh - maintained at 300 0-2C, or 950 020.
as required.
113.1.3 Th,'mDtnlUr - any convenient thermometer of a suitable
range. with 0-1 or 0-20 subdivisions. The thermometer should be
checked against a standard thermometer, which has been calibrated and
certified by the National Physical Laboratory, New Delhi, or any other
laboratory recognized for such work.
113.2 Proeldurl - Fill the bottle with the oil previously cooled to about
25 uC or the melted rat to overflowing, holding the' bottle on its side in
such a manner as to prevent the entrapment of air bubbles after' removing
the cap of the side arm. Insert the stopper, immerse in the water-bath
at 300 02C, or at 950 020, as required, aud hold for
30 minutes, Carefully wipe off B.ny oil which has come through the capillary opening. Remove the bottle from the bath, clean and dry it
thoroughly. Replace the cap of tile side arm, cool to room temperature
and weigh.
11.33 Cal,ulalion
A-B
40
FlO.
where
B
C
A _ B
b) Specific gravity
at
95C/30C
==
(C _ B) X [1
+ (0000025
65)]
where
A .. weight in g of the specific gravity bottle and fat at 9S oC,
B = weight in g of the specific gravity bottle,
C sa weight in g of the specific gravity bottle with water
at 300, and
0000 025 == coefficlent of expansion of glass.
11.3.4 C,me';tJIU - tl' 11.2.1.
41
to
300 ml capacity.
Liquid- mercury.
Filling above liquid- evacuated or nitrogen gas.
Tempera/ur, rangl -J1linus 2 to 680.
Subdivisions - O2C.
TOlallength - 385 to 390 mm,
Stem dimneter - 6 to 7 mm.
SlIm eonst;uetiDn - plain or lens front. The cross-section of
the lens front type shall be such that it will pus through an
8-mm ring gauge but will not enter a 5-mm slot gauge.
j) Bulb dillmtttr - from 5-5 mm to not greater than the diameter of
the stem.
k) Bulb lIng'"-
15 to 25 mm
42
2-lITRE lOW-FORM
BEAt<ER
CORK EQUAlLV SPACED
SAMPLE
TEST- TUBE
4S0-ml WIDE-MOUTH
BOTTLE
LEAD SHOT CR WEIGHl
f5
Flo. 8
TITRE TEST
rc
Un""
,1uImIJ"-
"_at;,,,
43
[""""n," -
12.2 ReageDu
12.2.1
PDtash Solu,ion - Dissolve with the aid of heat,
250 g of solid potassium hydroxide in I 250 g of glycerine. Do nOI: heat
above 140C.
12.2.2 Dilute Sulplwric Acid - 30 percent by weight obtained by
cautiously adding 16 ml of concentrated sulphuric acid, .p gr 184 [conforming to IS: 266-1961 Specification for Sulphuric Acid (Rnis,d)] to
70 mm of water.
12.23 Methyl Orang, Indicator Solution - Dissolve 01 g of methyl orange
in 100 ml of water.
12.2.4 Acetone - conforming to *IS: 170-1950 Specification for Acetone.
12.3 p ..ocecIare
123.1 Pr'!Jardtioft of Fatty Acids - Weigh about 70 g of the glycerolcaustic potash solution into the saponification flask. Heat to 150C while
stirring. Add about 30 g of the sample of oil or melted fat and re-heat to
about 150C. If necessary.. add a little more glvcerol-caustic potash solution to ensure complete saponification. ( Complete saponification is usually
indicated by an initial change in the appearance of the mass often
accompanied by an increase in the viscosity or thickening. The soluticn
then thins out after the reaction is complete 'and assumes a homogeneous
appearance. The most common characteristic is that of soap bubbles forming and rising from the surface. Considerable care should be exercised at
all tiJ?1e5 to ensure complete
CooI.lightly and
the
soap 10 300 lot of wacer contained 10 a I OOO-ml beaker. Add dalute sulphuric acid until the solution is distinctly acidic to methyl orange indicator,
and place the beaker in a boiling water-bath until the fatty acids coUect
as a clear layer at the top. Siphon off the lower aqueous acid layer, add
300 ml of hot water, place in the boiling water-bath for a few minutest and
again siphon off the aqueous acid layer. Wash the fatty, acids thrice in this
manner or until the last traces of soap and acid are removed. The
acidification and washing should be done in u short a period as possible,
keeping the beaker covered to prevent the oxidation of the fatty acids.
After the last wash, allow the fatty acids to settle fOr a few minutes and
then decant them carcfu!ly. Filter through one or two thicknesies of
Sinc. reviled.
44
45
13.3 Report - Report the colour of the oil in terms of Lovibond units as
follows:
Colour reading
in ( ) cell
==
+ 5 b R ) or ( a Y +
(G Y
lOb R )
where
13.3.2 The dimensions of the cell used and the mode of expressing the
colour reading for different oils shall he as follows:
outr
Si{,e-Designation
of Cell
( in )
Modi of Express;",
Colour Reddi,,&
Castor
Groundnut
Y+5R
Y+5R
Coconut
Y+ SR
Sesame
Mustard
MAHUA
I
i
Y +5R
Y+5R
Y+5R
( washed
and refined )
.Sizt desililation of the cell used.
46
Y+ lOR
14.1 Realeat.
14.1.1 Potassism Dichron,at' - conforming to IS : 250-1953 Specification
for Potassium Bichromate, Technical and Analytical Reagent,
to
IS: 265-1962
14.1.5 Standard Sodium ThiosulpluUe Solution - approximately 01 N. Dis101ve approximately 248 g of sodium thiosulphate crystals ( Na ISs03 , 51-1.0 )
in water which has been well boiled to free it from carbon dioxide and
make up to I 000 ml, Store the solution in a cool place in a dark.
coloured stock bottle with a guard-tube filled with soda lime, After storing
the solution for about two weeks, filter, if necessary, and standardize it as
prescribed under 14.1.5.1.
4903
Since revised.
47
J"
a:
48
or
IODDIa VALva
Eu&CT&D
WE.IGHING AccuaACY
-.A..
Maximum
(I)
U. than 3
14.2 )
Minimum
(2)
10
(4)
(3)
.0001
10
6-346 0
5-0770
10
31730
2-5384
50
0-661 2
0-5288
.0000 2
100
0317 3
0-2538
.0000 1
.0000 5
.0-000 2
150
0-212 5
0'1700
.0-000 1
200
0'158 6
0-1269
143 Calcal.doD
.
Iodine value
12'69 ( B - S) N
== ---w
-.-----
where
B == Volume in ml of standard sodium
required for the blank,
S == volume in ml of standard sodium
required for the sample,
N = normality of the standard sodium
and
W == weight in g of the material taken for
thiosulphate solution
thiosulphate solution
thiosulphate solution,
the test.
15.1 Apparata.
15.1.1 Conical Flasks - 250 to 300 ml capacity.
15.1.2
Condens" - any efficient reflux condenser, at least 65 em
long.
15.1.3 Water-Bath or Electric Hot-Plate with Rheostdt Control
15.2 Reale.t.
15.2.1 Alcoholic Potassium Hydroxide Solution - Dissolve 35 to 40 g of
potassium hydroxide in 20 rot of distilled water, and add sufficient
aldehyde-free rectified spirit [conforming to IS: 323-1959 Specification
for Rectified Spirit ( Revised) ] to make up to 1 000 ml. Allow to stand
. overnight, decant the clear liquid and keep in a bottle closed tight with a
cork or rubber stopper.
15.2.2.1 klethod 1- Redistil rectified spirit (conforming to IS: 3231959) over solid caustic soda or caustic potash, add 2 to 3 g of mttaphenylenediamine hydrochloride per litre of rectified spirit, digest at ordinary
temoerature for several days or under a reflux condenser on a steam-bath
for several hours and distil slowly) rejecting the first 100 ml and the last
200 ml of the distillate.
15.2.2.2 Method /1 - Reflux 1-2 litres of rectified spirit (confonning
to IS: 323-1959) for 30 minutes in a round-bottom flask with 10 g of
caustic potash and 6 g of granulated aluminium (or aluminium foil).
Distil and collect one litre after discarding the first 50 ml.
15.2.3 Phenolphthalein Indicator Solution - Dissolve 1-0 g of phenolphthalein in 100 rnl of rectified spirit ( conforming to IS: 323-1959 ).
NOTE- When testing oils or fats which give dark-eoloured soap lolutlOns, the
observation of the end point of the titration may be facilitated either <a> by ulin,
thymolphthalein, or alkali blue 68 in place oi phenolphthalein or (b) by adding one
millilitre bf a 0-1 percent ( rvlv) solution of methylene blue in water to each 100 m1 of
phenolphthalein indicator solution before the titratiol.
51
After the
flask and condenser have cooled somewhat, wash down the inside of the
condenser with about 10 ml of hot ethyl alcohol neutral to phenolphthalei-.
Add about one millilitre of phenolphthalein indicator solution, and titrace
with standard hydrochloric acid. Prepare and conduct a blank determinetion at the same time.
15.4 CalealadoD
..
561 (B - 9 \ N
Saponification value W L:.._
where
B
== volume
as
c:
16.1 Method A
16.1.1 A.'JHlrlJ,,"
16.1.1.1
long.
16.1.2 RtagentJ
16.1.2.1 Acetic anhydride - containing 95
follows:
53
under 15.3.
16.1.4 Calculation
a) Acetyl value ==
S'-s
}.OOO-O-OOO 15 S
S'-S
where
S' = saponification value after acetylation, and
16.2 MethOd B
16.2.1 Reagents
16.2.1.1 Pyridine - Reflux with powdered barium oxide and distil.
Use the fraction distilling above 114C.
16.2.1.2 Acetic anhydride
16.2.1.3 Acetylatin, agtnt- Mix one volume of acetic anhydride a.d
seven volumes of pyridine,
16.2.1.4 Alcoholic sodium laydroxitl, solut;,,. - Prepare by dissolving
sufficient aqueous caustic soda (60 percent wI") in 95 percent alcohol to
make a 030 to 035 N solution. Remove the precipitated carbonate by
filtering.
The solution should be standardized against standard acid in the
presence of phenolphthalein before use. The solution remains colourless
for a long time if kept below 25C.
16.2.1.5 Normal butyl alcohol
16.2.1.6 Phtnolp1JI"alti" solution - Dissolve 01 g in 100 ml of 60 percent rectified spirit.
Non - In the determination upon lubitaDces Bivinl dark-eoloured IOAp IOIutiou,
observation of the end point of the titration may be facilitated either (a) by the
54
CalculatiDn
a) Hydroxyl value, H =
b) Acetyl value, A
=a
56'1 NY
W
H
+ 0'000 75 fj
55
r-
-a+6-,
where
17.1 Apparata.
17.1.1 DistiUation FI4Sk - SOO-ml round-bottomed flask.
17.1.2 Any Ejfiaen' Rtftux Cotlturuer- approximately 90 em long.
17.1.3 MetJSllri", Flask-200 ml capacity.
17.1.4 Waln-Batla
17.2 RealeDt.
17.2.1 E'k)l Alcohol- 95 percent (by volume) or rectified spirit (con-
5&
17.4 CalealatioD
Allyl
by weight
percent
9915 ( B - S) N
== .
W
where
S20!S
,10 Inl
100 rnl
59
----..t
_.- ----+--
J75!2500
Fro. 10
flame from impinging on the surface of the flask above the hole.
A new asbestos beard may conveniently be prepared by bevelling
the edge of the hole, soaking in water, moulding the edge with a
flask, and drying.
f) Bunsen Barner - The burner (F) should be sufficiently large
to allow the distillation to be com pleted in the time specified
in 18.3.2.
18.2
18.2.1 Glycerine - conforming to AR Grade of IS: 1796-1960 Speci..
fication for Crude Glycerine and Refined Glycerine.
Hydroxide
Dissolve sodium hydroxide in an equal weight of water and store the solution in a bottle protected from carbon dioxide. Use the clear portion free
from deposit.
18.2.3 Pumice Stone Grains - approximately 14 to 2'0 mm in diameter.
18.2.4 Dilut Sulphuric A.cid Solution - approximately 10 N.
18.3 Procedure
18.3.1 Weigh accurately 5-00 001 g of the filtered oil or fat into the
boiling flask. Add 20 g of glycerine and 2 ml of the concentrated sodium
hydroxide solution from a burette to which access of carbon dioxide is
prevented and whose orifice is wetted before running in the liquid, the
first few drops from the burette being rejected. Heat the flask and its
contents with continuous shaking on a gauze over the naked flame until
the fat, including any drops adhering to the upper parts of the flask. hac;
been saponified and the liquid becomes perfectly clear. Avoid overheating
during this saponification. Cover the flask with a watch.. glass. and a 110\\the flask to cool a little. Add 90 ml of boiling distilled water which has
been vigorously boiled for about 15 minutes. After thorough mixing, the
solution should remain clear. If the solution is not clear ( indicating incomplete saponification) or is darker than light yellqw (indicating overheating ),
r epeat the saponification with a fresh sample of the oil or fat. If the
is old. the solution may sometimes be dark and not clear.
60
for 10 minutes, making sure that the IIO-ml graduation mark is below the
level of the water. Swirl round the contents of the flask from time to time.
Dry the outside of the flask and then mix the distillate by closing the flask
and inverting it four or five times, but do not shake.
Filter through a dry
9-cm Whatman No.4 filter paper. Reject the first 2 or 3 ml of the filtrate
and collect the rest in a dry flask.
Non - The filtrate should 1-.,. free from insoluble Catty acids. When operatins on
coconut oil, it hu been noticed that this is not easily achieved. In cases where liquid
inlOluble Catty acids pass through the filter, transfer the filtrate to a separating (unnel
and after the separation of the lower aqueous layer, add the insoluble acids to the maiD
bulk of insoluble acicb.
61
IS I
( Part I )-1964
high altitudes. that ii, low barome:tric presluft:l. the Reichert-Meill. value determination. are lower than those determined at atmospheric presaure. The correction formulae
suggested by Kirkham were verified by Fine.
Since the Reichert-Meiss) value varies with atmospheric prellUre, correction. (or the
value arc necessary when the determinations are made at places above lea-level or when
barometric pressure it ftuctuating widely from 760 mm. The corrected Rcichert--Meiul
value sball be calculated .. follows;
ReichertMellll value
== -10"1,---+10
where
determination.
19. DETERMINATION
or
POLENSKE VALUE
19.0 General - The condenser, the 25-ml cylinder and the receiver used
in the Reichert-Meissl value determination are washed into the filter paper
through which the distillate was filtered for that determination,
After
rinsing, the residue on the filter paper is taken up with ethyl alcohol and
titrated with standard sodium hydroxide solution.
11.1 Reagents - All the reagents required for determining the ReichertMeissl value ( see 18.1 ) as well as the following are required.
percent by
volume,
and
neutral
to
19.2 Apparatus - the same apparatus as that required for the determination of Reichert-Meiss] value ( see 18.2 ).
19.4 Calca1atioD
Polenske value
62
lID
10 VN
where
py - observed Polenlke value, and
or
or
20.1 o.tUa.
the Methocl _. The rnarerial in an acetic acid-chloroform
medium, is treated with an aqueous solution of potassium iodide. The
liberated iodine is titrated with standard sodium thiosulphate solution.
W.2 Apparata.
20.2.1 Pi",t,. - Graduated. 1 ml capacity.
20.'.2 PoJ4Ssillm
Iodide Solution - Saturated.
Prepare saturated
solution of potassium iodide in recently boiled distilled water. Store
in the dark.
20.4_
a.t.l
500 005 g of sample of rat in a 250-ml II...
stoppered conical flask and then add 30 ml of the acetic acid-chloroform
IOlution. Swirl the flask until the sample is dissolved. Add 05 ml of
saturated potassium iodide solution. Allow the solution to stand
exactly one minute with occasional shakin(J and then add 30 ml or
distilled water. Titrate with 01 N sodium thiosulphate solution with can.tant and vigorous shaking. Continue titration until the yellow colour
almOit disappean. Add 0-5 ml of starch solution and continue titration
till the blue colour just disappcan.
2O.t.2 If the titre value is leu than 0'5 ml, repeat the determination
using 0-01 N sodium thiosulphate lolution.
20.43 Conduct a blank determination of the reagents in the same way.
The titration in blank determination should not exceed 0-1 m1 of the
0-1 N sodium thiosulphate solution.
20.5 Calcaladoa - Peroxide value as milli-equivalents per I 000 gramJ
sam I
(S-B)xNxIOOO
pe -
where
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TO
IS 548 ( Part 1 ) : 1964 METHODS OF SAMPLING AND
TEST FOR OILS AND FATS
PART 1 SAMPLING, PHYSICAL AND CHEMICAL TESTS
(Revised)
'16.2.3.2 Mix the rat and the acetyIating agent by shaking well. Add one or two
small pieces of pumice stone and beat tbe contents of the flask on steam-bath
under reflux condensorfor 60 minutes.'
.
(FAD 44 )