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Indian Standard: Specification For Amyl Acetate

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IS : 231 - 1957

(Reaffirmed 2001)
( Reaffirmed 2005 )
Edition 1.2
(1975-06)
Indian Standard
SPECIFICATION FOR
AMYL ACETATE
(Incorporating Amendment Nos. 1 & 2)

UDC 66.062.612.15

© BIS 2002

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN , 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Price Group 5
IS : 231 - 1957

Indian Standard
SPECIFICATION FOR
AMYL ACETATE
Fine Chemicals (Organic & Inorganic) Sectional Committee, CDC 4
Chairman
DR J. N. RAY Directorate General of Industries and
Supplies, New Delhi
Members
SHRI N. ADHIKARI Bengal Chemical & Pharmaceutical Works
SHRI AMIYA KUMAR LAHIRI ( Alternate ) Ltd, Calcutta
DR J. C. BARDHAN College of Science & Technology, University
of Calcutta, Calcutta
DR U. P. BASU Bengal Immunity Co Ltd, Calcutta
DR L. A. BHATT Kesar Sugar Works Ltd, Bombay
SHRI J. FRASER DUFF Textile Chemistry Sectional Committee
SHRI W. E. WILKIE-BROWN ( Alternate ) (TDC 5)
SHRI F. W. GRIFFIN British Drug Houses (India) Ltd, Bombay
SHRI E. H. BALDOCK ( Alternate )
DR K. A. HAMIED Chemical, Industrial & Pharmaceutical
SHRI AJOY GUPTA ( Alternate ) Laboratories Ltd, Bombay
DR B. D. LAROIA Council of Scientific & Industrial Research,
New Delhi
SHRI B. MAITRA Indian Chemical Manufacturers’
Association, Calcutta
SHRI S. S. MEHTA Indian Tariff Board, Government of India,
Bombay
SHRI P. M. NABAR Directorate General of Health Services,
SHRI P. S. RAMACHANDRAN ( Alternate ) Ministry of Health, New Delhi
SHRI S. RAMABHADRAN Directorate of Technical Development,
Army Headquarters, New Delhi
DR LAL C. VERMAN ( Ex-officio ) Director, ISI
Staff
DR K. L. MOUDGILL Indian Standards Institution

( Continued on page 2 )

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN , 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
IS : 231 - 1957

( Continued from page 1 )

Alcohols and Esters Subcommittee, CDC 4 : 2

Convener
DR B. D. LAROIA Council of Scientific & Industrial Research,
New Delhi
Members
SHRI B. MAITRA Calcutta Chemical Co Ltd, Calcutta
SHRI J. N. RAKSHIT ( Alternate )
SHRI S. RAMABHADRAN Directorate of Technical Development,
Army Headquarters, New Delhi
SHRI J. P. SHUKLA Rampur Distillery & Chemical Co Ltd,
Rampur
Staff
SHRI K. VYASULU Indian Standards Institution

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IS : 231 - 1957

Indian Standard
SPECIFICATION FOR
AMYL ACETATE
FOREWORD
This Indian Standard was adopted by the Indian Standards
Institution on 27 October 1950 as a tentative standard on the
endorsement by the Chemical Division Council of the draft finalized
on 25 August 1950 by the Fine Chemicals (Organic & Inorganic)
Sectional Committee. In June 1957, this standard was issued as firm
Indian Standard without any modification.
This standard prescribes the requirements for technical and pure
grades of amyl acetate. In laying down the requirements of amyl
acetate, technical, note has been taken of the fact that this material is
supplied in the market from two sources viz, synthetic and, fusel oil.
In the preparation of this standard, considerable assistance was
derived from the standards of the American Society for Testing
Materials, the British Standards Institution and the Standards
Association of Australia and the help derived from these sources is
acknowledged.
This standard is intended chiefly to cover the technical provisions
relating to the purchase of the material, and it does not include all the
necessary provisions of a contract.
This edition 1.2 incorporates Amendment No. 2 (June 1975). Side
bar indicates modification of the text as the result of incorporation of
the amendment.

1. SCOPE
1.1 This standard prescribes the requirements and the methods of
test for Amyl Acetate, Technical and Pure. Amyl acetate, technical, is
used mainly as a solvent by the paint, varnish and lacquer industry,
and amyl acetate, pure, is used as a flavouring material in perfumes
and in photo-engraving and as a laboratory reagent.
2. GRADES
2.1 There shall be two grades of amyl acetate, namely, Technical and Pure.
3. SAMPLING
3.1 Representative samples of the material shall be drawn as
prescribed in Appendix A.
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IS : 231 - 1957
4. REQUIREMENTS
4.1 Unless specified otherwise, chemicals of the purest grade shall be
employed in the tests and distilled water shall be used where the use
of water as a reagent is specified.
4.2 Description — Amyl acetate, technical or pure shall be a clear,
colourless liquid, free from visible impurities.
4.3 Freedom from Water — No trace of opalescence shall be
produced when 1 volume of the material is mixed, at 15ºC, with
19 volumes of carbon disulphide.
4.4 The material shall also comply with the requirements in Table I,
when tested according to the methods prescribed in the appendices
referred to in column (5) of the table.
4.5 Special Requirement — When the material is required for use
in pyrotechnic industry, it shall also comply with the requirement of
moisture content 0.3, percent, Max when tested by the method
described in IS : 2362 - 1963 Determination of Water by the Karl
Fischer Method.

TABLE I REQUIREMENTS FOR AMYL ACETATE


SL CHARACTERISTIC REQUIREMENT FOR GRADE METHOD OF
NO. TESTING (REF















Technical Pure TO APPENDIX)
(1) (2) (3) (4) (5)
i) Specific gravity at 20/20ºC 0.857 to 8.870 0.868 to 0.876 B
ii) Residue on evaporation, 0.02 0.01 C
percent by weight, Max
iii) Acidity, calculated as acetic 0.03 0.01 D
acid, percent by weight,
Max
iv) Ester content, percent by 85 97 E
weight, Min
v) Range of distillation 100 ml of amyl 100 ml of amyl F
acetate shall yield acetate shall yield
on distillation at on distillation at
760 mm pressure 760 mm pressure
not less than not less than
85 ml between 95 ml between
125 and 145ºC 125 and 145ºC

5. PACKING AND MARKING


5.1 The material shall be supplied, in accordance with the marking
and delivery instructions given by the purchaser, in leak-proof
containers approved by the purchaser.

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IS : 231 - 1957
5.2 Each container shall be marked with the name of the
manufacturer, the grade and weight of the material in the container,
recognized trade mark, if any, and the month and year of manufacture.

APPENDIX A
( Clause 3.1 )
SAMPLING OF AMYL ACETATE

1. GENERAL REQUIREMENTS OF SAMPLING


1.0 In drawing, preparing, storing and handling test samples, the
following precautions and directions shall be observed.
1.1 Samples shall be taken in a protected area with good ventilation.
1.2 The sampling instrument shall be clean and dry when used.
1.3 The samples, the material being sampled, the sampling
instrument and the containers for samples shall be protected from
adventitious contamination.
1.4 To draw a representative sample, the contents of each container
selected for sampling shall be mixed as thoroughly as possible by
shaking or stirring or rolling or by any other suitable means so as to
bring all portions into uniform distribution.
1.5 The samples shall be placed in clean, dry and air-tight glass or
metal containers on which the material has no action.
1.6 The sample containers shall be of such a size that they are almost,
but not completely, filled by the sample.
1.7 Each sample container shall be sealed air-tight with a suitable
stopper after filling and marked with the manufacturer’s name or
trade-mark, grade of the material, the month and year of manufacture
of the material, the batch number (if available) and other details of
sampling, such as the date of sampling, sampler’s name, etc.
1.8 Samples shall be stored in such a manner that the temperature of
the material does not vary unduly from the normal temperature.

2. SAMPLING INSTRUMENT
2.1 Sampling Tube — It is made of thick glass or metal on which the
material has no action and is 20 to 40 mm in diameter and 400
to 800 mm in length ( see Fig. 1 ).

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IS : 231 - 1957

FIG. 1 SAMPLING TUBE


The upper and lower ends are conical and reach 5 to 10 mm diameter
at the narrow ends. Handling is facilitated by two rings at the upper
end. For drawing sample, the apparatus is first closed at the top with
the thumb or a stopper and lowered till a desired depth is reached. It
is then opened for a short time to admit the material at the desired
depth and finally closed and withdrawn.
2.1.1 For small containers, the size of the sampling tube may be
altered suitably.
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IS : 231 - 1957
3. SCALE OF SAMPLING
3.1 Lot — In any consignment, all the containers of the same grade
and size, drawn from the same batch of manufacture, shall constitute
a lot. If a consignment consists of containers of different grades, or of
different batches of manufacture or of different sizes, the containers
belonging to the same grade, batch and size shall be grouped together
and each such group shall constitute a separate lot.
3.2 For ascertaining the conformity of the material in a lot to the
requirements of this specification, tests shall be carried out for each
lot separately. The number of containers to be selected for this
purpose from a lot shall depend on the size of the lot and shall be in
accordance with col 1 and 2 of Table II.

TABLE II SCALE OF SAMPLING


LOT SIZE NO. OF CONTAINERS TO BE
SELECTED
N n
(1) (2)
Up to 3 *
4 ,, 15 3
16 ,, 40 4
41 ,, 65 5
66 ,, 110 7
111 ,, 180 8
181 ,, 300 9
301 and above 10
*In case the lot consists of 3 or less than 3 containers, the number of containers to be
selected and the method of judging the conformity of the lot to the specification
requirements shall be as agreed to between the purchaser and the supplier.

3.3 Containers shall be selected at random from the lot and, in order
to ensure randomness of selection, a random number table as agreed
to between the purchaser and the supplier shall be used. In case such
a table is not available, the following procedure is recommended for
use:
Arrange all the containers in the lot in a systematic manner and
starting from any container count them as 1, 2. . . up to r and so on,
where r is the integral part of N/n ( N being the lot size and n, the
number of containers to be selected ). Every rth container thus
counted shall be withdrawn to constitute the sample.

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IS : 231 - 1957
4. PREPARATION OF TEST SAMPLES
4.1 From each of the containers selected according to 3.3, a
representative portion of the material, sufficient for carrying out the
tests specified under REQUIREMENTS shall be drawn with the help
of the sampling tube ( see 2.1 ).
4.2 Out of these portions, equal quantity of material shall be taken
and mixed thoroughly to form a composite sample, not less
than 1 500 ml. The composite test sample shall be divided into 3 equal
parts, one for the purchaser, another for the supplier and the third to
be used as a referee sample.
4.3 The composite samples shall be transferred to containers of
600 ml capacity and shall be sealed and marked with full
identification particulars given in 1.7.
4.4 The referee test sample shall also bear the seal of both the
purchaser and the supplier. It shall be kept at a place agreed to
between the purchaser and the supplier, to be used in the case of any
dispute between the two.
5. CRITERIA FOR CONFORMITY
5.1 The lot shall be declared as conforming to the standard, if the test
results of the composite test sample satisfy the requirements
prescribed under REQUIREMENTS. Otherwise the lot shall be
rejected.

APPENDIX B

[ Table I, Item (i) ]


DETERMINATION OF SPECIFIC GRAVITY

1. DEFINITION
1.1 For the purposes of this standard the specific gravity of the
material is the ratio of the weight of a given volume of the material to
that of an equal volume of distilled water, the temperature of both the
material and the water being 20ºC.

2. APPARATUS
2.1 A specific gravity bottle of about 50 ml capacity.

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IS : 231 - 1957
3. PROCEDURE
3.1 Clean, dry and weigh the bottle and the cap. Fill with water,
introduce the cap and keep it at a temperature of 20ºC for 15 minutes.
Suck off the water with a bit of filter paper, till the level reaches the
graduation mark, and weigh again. Empty the bottle, clean and dry it,
and repeat the operations with the material.
3.2 Calculation and Report — The temperature of testing shall be
specified in the report.
c–a
Specific gravity = ------------
b–a
where
a = weight of the dry specific gravity bottle.
b = weight of the specific gravity bottle filled with distilled water,
and
c = weight of the specific gravity bottle filled with the material.

APPENDIX C
[ Table I, Item (ii) ]
DETERMINATION OF RESIDUE ON EVAPORATION

1. PROCEDURE
1.1 Evaporate 100 ml of the material, accurately measured into a
tared nickel, silica or hard glass basin of about 75 mm diameter and
20 mm deep. Dry the residue for one hour at 150 ± 2ºC. Cool the
residue in a desiccator and weigh.
1.2 Using the specific gravity of the material determined under
Appendix B, calculate the residue on evaporation as percentage of the
weight of the material taken.
B–A
Residue on evaporation, percent = --------------
S
where
A = weight of empty basin,
B = weight of basin after evaporation and drying, and
S = specific gravity of the material.

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IS : 231 - 1957

APPENDIX D
[ Table I, Item (iii) ]
DETERMINATION OF ACIDITY

1. REAGENTS
1.1 Phenolphthalein Indicator — Dissolve 0.5 g of
phenolphthalein in 100 ml of 95 percent ethyl alcohol and make the
solution faintly pink by adding sodium hydroxide solution.
1.2 Standard Sodium Hydroxide Solution — approximately
0.01 N.
2. PROCEDURE
2.1 Mix 20 ml of the ester, delivered from a pipette, with 20 ml of
neutral alcohol and titrate the mixture with standard sodium
hydroxide solution using 0.5 ml of phenolphthalein indicator.
3. CALCULATION
3.1 Using the specific gravity determined under Appendix B, calculate
the acidity as percentage by weight on the basis that 1 ml of 0.01 N
sodium hydroxide solution is equivalent to 0.000 6 g of acetic acid.

APPENDIX E

[ Table I, Item (iv) ]


DETERMINATION OF ESTER CONTENT

1. REAGENTS
1.1 Standard Alcoholic Sodium Hydroxide — approximately 0.5 N.
1.2 Standard Hydrochloric Acid — approximately 0.5 N.
1.3 Phenolphthalein Indicator — prepared as in 1.1 of Appendix D.

2. PROCEDURE
2.1 Weigh accurately 1 to 1.5 g of the ester in a small, stoppered, tared
tube, and transfer the tube with its contents to a flask containing 50 ml of

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IS : 231 - 1957
alcoholic sodium hydroxide solution. Fit a water-cooled reflux condenser
to the flask and heat the latter for one hour over a boiling water bath. At
the end of the heating period, rinse the condenser with well-boiled and
cooled distilled water. Cool, remove the flask and titrate the contents with
standard hydrochloric acid, using 0.5 ml of phenolphthalein indicator.
2.2 Carry out a blank determination, using all the materials excepting
the ester, under similar conditions and at the same time.
3. CALCULATION
3.1 From the difference in the volumes of standard sodium hydroxide
required in the titrations with and without the material, and using
the factor that 1 ml of 0.5 N alcoholic sodium hydroxide is equivalent
to 0.065 of amyl acetate, calculate the weight of the ester for 100 g of
the material.

APPENDIX F
[ Table I, Item (v) ]
DETERMINATION OF RANGE OF DISTILLATION

1. APPARATUS
1.1 Distillation Flask — of the shape and dimensions given in Fig 2.
Fix the flask in the vertical position by means of a clamp at the
extreme upper end of the neck.
1.2 Thermometer — so fitted in the flask that the bottom of the
capillary is level with the lower edge of the side-tube joint and the
immersion mark is level with the top of the cork.
1.2.1 The recommended dimensions, tolerances and graduations of
the thermometer shall be as follow:
Range 90 to 160ºC
Graduation 0.2ºC
Longer lines at each 1ºC
Fully figured at each 5ºC
Immersion 100 mm
Overall length 315 to 325 mm
Length of main scale, not less than 170 mm
Bulb length, not greater than 15 mm
Stem diameter 5 to 6.5 mm

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IS : 231 - 1957
Distance from the bottom of bulb to 100 to 125 mm
bottom of main scale
Distance from the bottom of bulb to top of 25 mm
contraction chamber, not greater than
Maximum error 0.8ºC
Maximum error in an interval 0.8/10ºC

FIG. 2 DISTILLATION FLASK


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IS : 231 - 1957
1.2.2 The thermometer shall bear a certificate of the National
Physical Laboratory of India or any other institution authorized by
the Government of India to issue such a certificate.
1.3 Rectangular Draught Screen — made of 0.710 mm thick sheet
metal, with the dimensions shown in Fig. 3 and open at the top and
bottom, fitted with hard asbestos or silica board, with a central hole
100 mm in diameter. It shall comply with the following requirements.
1.3.1 In each of the two narrow sides of the draught screen there shall
be two circular holes, each 25 mm in diameter, and in each of the four
sides of the draught screen there shall be three holes with their
centres 25 mm above the base of the draught screen. These holes shall
occupy the positions shown in Fig. 3, the diameter of each of the holes
centrally situated in the longer sides shall be 25 mm and, of the
remaining ten holes, shall be 12.5 mm. At the middle of each of the
wider sides a vertical slot with the dimensions shown in Fig. 3 shall be
cut downwards from the top of the screen.
1.3.2 A sheet of hard asbestos, 6 mm in thickness, and having a
central circular hole, 50 mm in diameter, shall be supported
horizontally in the screen and shall fit closely to the sides of the screen
to ensure that hot gases from the source of heat do not come in contact
with the sides or neck of the flask. The supports for this asbestos sheet
may conveniently consist of triangular pieces of metal sheet firmly
fixed to the screen at its four corners.
1.3.3 In one of the narrow sides of the screen a door shall be provided
having the dimensions and position as shown in Fig. 3. In each of the
narrow sides of the screen a mica window shall be placed centrally,
with the bottom of the window on a level with the top of the asbestos
shelf. The dimensions and position of the windows are shown in Fig. 3.
1.4 Liebig Condenser — with the bent end made of good quality
resistance glass, with a wall thickness of 1 to 1.5 mm and conforming
to the shape and dimensions given in Fig. 4.
1.4.1 Alternatively, the bent portion may be substituted by an adapter
fitted externally in such a manner that the distillate does not come in
contact with the cork.
1.5 100 ml Crow Receiver (Fig. 5) or Graduated Cylinder — with
millilitre marks running halfway round the circumference, with
5 millilitre marks running three-quarters-way round, and with
10 millilitre marks running all round the circumference, and numbered.
1.6 Bunsen Burner — giving an entirely non-smoky flame and
provided with an adjustable screw clip with the help of which the
flame can be lowered or raised according to requirement.
1.7 Half-Second Pendulum — for measuring the rate of distillation.
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IS : 231 - 1957
14

FIG. 3 DRAUGHT SCREEN


IS : 231 - 1957

FIG. 4 LIEBIG CONDENSER

FIG. 5 100 ml CROW RECEIVER


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IS : 231 - 1957
2. PROCEDURE
2.1 Assemble the apparatus as shown in Fig. 6. Measure 100 ml of the
material at laboratory temperature into the 100 ml Crow receiver and
transfer it to the distillation flask, the contents of the receiver being
allowed to drain for fifteen seconds into the flask. Add a fragment
(about 2 mm cube) of porous pot or other suitable inert material to
prevent bumping, connect the flask to the condenser and insert the
thermometer. Pass an adequate supply of cooling water through the
condenser. To receive the distillate, use the Crow receiver in which
the sample was measured, without rinsing or drying. Heat the flask
slowly, especially after ebullition has begun, in order that the mercury
column of the thermometer may become fully expanded before the
first drop of distillate falls into the receiver, care being taken that the
total period of this preliminary heating shall be not less than five nor
greater than ten minutes. Place the receiver so that the condensate
will flow down its side. Continue the distillation at the rate of 4 to
5 ml per minute (about 2 drops per second). Read the volume of
distillate in the receiver when the thermometer indicates each of the
specified distillation temperatures, the temperatures on the
thermometer scale being corrected as specified under 3. The difference
between the volumes so recorded is the percentage by volume
distilling between the specified temperatures at 760 mm pressure.
3. CORRECTION OF THE THERMOMETER READING
3.0 The following corrections shall be applied before starting
distillation.
3.1 Error of Scale — In all thermometer reading, make the
corrections as indicated on the certificate of the instrument.
3.2 Correction for Barometric Pressure — If the barometric
pressure prevailing during the determination is normal, namely
760 mm of Hg, no correction need be applied to the specified
temperature, and the thermometer scale as corrected under 3.1 may
be used as such. If the prevailing barometric pressure deviates from
760 mm, the specified temperature shall be corrected as follows and
used on the thermometer scale as corrected under 3.1.
3.2.1 For every 10 mm above 760 mm add 0.43ºC to the specified
temperature and for every 10 mm below 760 mm subtract 0.43ºC from
the specified temperature. These corrections shall be applied in
proportion at the above rate for any prevailing barometric pressure
and are valid down to a pressure of 700 mm of Hg.

16
17

FIG. 6 ASSEMBLY OF APPARATUS

IS : 231 - 1957
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promote harmonious development of the activities of standardization, marking and quality
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Review of Indian Standards
Amendments are issued to standards as the need arises on the basis of comments. Standards are
also reviewed periodically; a standard along with amendments is reaffirmed when such review
indicates that no changes are needed; if the review indicates that changes are needed, it is taken up
for revision. Users of Indian Standards should ascertain that they are in possession of the latest
amendments or edition by referring to the latest issue of ‘BIS Catalogue’ and ‘Standards : Monthly
Additions’.
This Indian Standard has been developed by Technical Committee : CDC 4 and amended by CDC 2

Amendments Issued Since Publication


Amend No. Date of Issue
Amd. No. 1 Incorporated earlier
Amd. No. 2 June 1975

BUREAU OF INDIAN STANDARDS


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