Professional Documents
Culture Documents
Indian Standard
SPECIFICATION FOR ACETONE
( Third Revision )
Second Reprint OCTOBER 1998
UDC
661.727.4
3anmaty 1987
IS : 170 - l!m6
Indian Standard
SPECIFICATION ( FOR ACETONE
Third Revision )
Sectional Committee, PCDC 10
Reprcscnfing Union Carbide India Ltd, Calcutta
Forensic Science Laboratory; and Chemical Analyser to the Government of Maharashtra, Bombay
SHRI K. C. SAH ( Altcrnafs 1 to Dr R. B. Roy Choudhry ) SHRI V. R. DUBEY ( Alfanafr II to Dr R. B. Roy Choudhry ) DR S. K. ME~HAL ( Alfernafc to Dr B. N. Mattoo ) National Organic Chemical Industries Ltd, SHRI K. D. APRE Bombay SERI P. CHAWLA ( Alternate ) Polychem Ltd, Bombay SHRI WILSON D. ANDRAT DR R. C. DIKSHIT ( Altwnatc ) Ministry of Defence ( DC1 ) SHRI J. A. ASETAPUTRE Snnr P. K. MAZU~DAR ( Altcrnafc ) Indian Organic Chemical Industries Ltd, Kopoli SHRI R. A. BAKSHI SHRI S. H. KILLEDAR ( Affernafs ) SHRI R. A. BAKSHI Indian Chemical Manufacturers Association Calcutta SHRI P. R. MAHALIN~AM ( Alternate ) SHRI 0. P. B~ATIA All India Distillers Association, New Delhi SHRI P. N. SAPRA ( Alfcrnafc) DR G. S. CHAUDHARI Directorate of Health Services, Lucknow CHIEF CHEMIST Central Revenues Control Laboratory, New Delhi DEPUTY CHIEF CHEMIST ( Affernafc ) SHRI H. C. CEIOP~A Synthetic & Chemicals Ltd, Bombay SHRI R. N. MEHROTRA ( Alfernafe ) DR D. K. DAS National Test House, Calcutta SHRI N. C. CHATTERJEE ( Alternate ) SHRI R. C. GUPTA Directorate General of Technical Development New Delhi SH~I S. N. PANDEY ( Alternate ) ( Con&ucd on page 2 ) Q Co#prighf 1987 BUREAU OF INDIAN STANDARDS This publication is protected under the Indian Copvrighf Acf ( XIV of 1957 ) and reproduction in whole or in part by any means except with written permission of the publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 170 - 1986
pagr 1 ) Rcpresenfing Members Mohan Meakin Breweries Ltd, Ghaziabad Sam E. K. JAYANARAYANAN Snnr JITENDRA MORAN ( Alternate ) Hindustan Polymers Ltd, Bombay SERI S. K. MAEAJAN SHRI A. K. MUKHERJEE ( Altcrnafe ) Herdillia Chemicals Ltd, Bombay DR J. RAJARAM Sang V. G. FADNIS ( Alternate ) The Alkali & Chemicals Corporation of India Ltd, SHRI R. SANTHANAM Calcutta SARI S. C. TALAPATRA ( Altcrnalc ) The Sir Silk ltd, Hyderabad Sam D. R. K. SAYOJI RAO Saur SREEDHARAN ( Alternate ) Central Forensic Science Laboratory, New Delhi DR V. N. SEHGAL DR V. S. BISARIA ( Alternate ) The Indian Drugs and Pharmaceuticals Ltd, SHRI SURENDRA SJNQH Muzaffarpur Snnr R. K. BANDOPADEYAYA ( Alternate ) Somaiva ( India ) Ltd, Barabanki Dn S. K. S~MAIYA , Organic SARI H. B. DESAI ( Alfsrnafc ) Ministrv of Chemicals and Fertilizers, New Delhi DR MOHAIMED SWALEH State Forensic Science Laboratories, Government SHRI 0. P. TANEJA of Uttar Pradesh, Lucknow National Sugar Institute, Kanpur DR L. VISHWANATHAN Director General, IS1 ( Ex-oficio Member ) Sam M. S. SAXF,NA, Director ( P&C )
( Conrinwrffiom Secretary SHRI M. A. U. KHAN Joint Director ( P & C ), ISI
PCDC
10 : P3
Corw8ner JOSEPH
SHRI K. C. SAH ( Alternate to Shri V. D. Joseph ) SHRI K. D, AYRE .s~I V. K. PAI~AM~SWAR,\ AYY.\R _____.
SHRI P. CHAWLA ( Allsrnale
Chemicals
Industries
Ltd,
SARI H. B. DESAI DR R. B SRIVASTAVA ( Alhrnalc SHRI R. v. &KnAr,E Snur A. A. INA?XDAR Snur P. S. RA~~ANAT~AN SRRI V. C. Saui~a ( Alternate ) SHnI T. N. RAwAL Snnr P. N. AQARWAL ( Alternate
SHRX G. B. SHAH ( Alfrr rote ) Vam Organic DR S. C. I~IRAI~YA SHHI YOGENDRA KTJMAIS ( Alfcrnafc )
Ltd, Gajraula
Somaiya Organics ( India ) Ltd, Barabanki ) Herdi lia Chemicals Ltd, Bombay Hico Products Ltd, Bombay Indian Drugs 8t Pharmaceuticals Ltd, Muzaffarpur ( DGI )
Ministry of Defence )
IS:170-
1986
Indian Standard
SPECIFICATION FOR ACETONE
( Third Revision)
0. FOREWORD
0.1 This Indian Standard ( Third Revision ) was adopted by the Indian Standards Institution on 30 June 1986, after the draft finalized by the Alcohols and Allied Products Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council. 0.2 This standard was first issued in 1950 and subsequently revised in At the time of first revision, a comparative study of the 1966 and 1976. standard with the draft IS0 Recommendation No. 656 Sampling and methods of test for acetone was undertaken. A revised scheme of sampla new procedure for determination of inq and criteria for conformity, ;i!coholic impurities, refinement in the test for alkalinity and additional rcquircrncnt for water contrnt were included in the revised standard. As a rc.sriit of experience gained through the use of first and second revisions and in order to meet the present day requirements of acetone, this third revision has been undertaken in which limits for colour, water content and pcrmanganate test have been modified. 0.3 Acetone is an important commercial solvent and raw material with a wide usage in the chemical, explosives and iacquer industry. It is commonIv used as a solvent for cellulose acetate; nitrocellulose; celluloid; ccl~u~osr ether; chlorinated rubber; various resins, fats and oils; and as an absorbent for acetylene. It is being increasingly used in the synthesis of a number of chemicals such as diacetone alcohol, methyl isobutyl methyl methocrylate and certain resins, kctonc, phorone, isophorone, pharrnncr:uticals and perfumes. requirement of this 0.4 For the purpose of decidin g whether a particular standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS : 2-1960*. The number of significant places retained in the rounded off value should br the same as that of the specified value in this standard. *Ilr~les
( revised ).
IS : 170 - 1986 1. SCOPE 1.1 This standard prescribes the requirements, methods test for acetone intended for industrial purposes. 2. REQUIREMENTS 2.1 Description -The material shall be clear and free from any suspended matter. It shall consist essentially of 2-propanone or dimethyl ketone ( CH&OCHS ). 2.2 Miscibility with Water - The material shall show no turbidity mixing with distilled water in any proportion at 27 f 2C. 2.3 The Table 1. material AND shall also comply with the requirements given on in of sampling and
3. PACKING
MARKING in sound and clean coninstructions given by the legibly and indelibly
3.1 Packing - The meterial shall he supplied tainers according to the marking and delivery purchaser. 3.2 Marking Each container with the following information: a) Name c) e) of the material; name; trade-mark, if any; and
shall be marked
b) Manufacturers d) Recognized
Net, gross and tare mass; Date of packing. with the minimum cautionof
3.2.1 Each container shall also be marked ary notice worded as FLAMMABLE. 3.2.1.1 It shall also dangerous goods [see Fig.
NOTEI-Necessary safeguards against the risk arising from storage and handling oflarge volumes of flammable liquids shall be provided and all due precautions shall be taken at all times to prevent accidents by fire or explosion ( scc 1s : 74451974+ ).
NOTE 2 - Except when they are opened for the purpose of cleaning and rendering them free from acetone vapour, all empty tanks or other containers shall be kept securely closed unless they have been cleaned and freed from acetone vapour. *Pictorial markings for handling (first revision ) . tCode of safety for acetone. and labelling of goods: Part 1 Dangerous goods
IS:170 - 1986
TABLE 1 REQUIREMENTS ( Clause 2.3 ) SL CHAEACTERISTIC REQUIIXEMENT MXTHOD or TEST, REB TO c--.---*-------~ Cl No. in Appendix of Indian Standard This Standard (4) A by anyother suitable instrumental method ii) iii) Relative 27127C Distillation density range
at
FOR ACETONE
(1)
i) Colour,
(2)
MUX
(5) -
O-784 to 0786 The difference between initial boiling point ( IBP ) and dry point(DP) shall not exceed 1C including 561C ( temperature being corrected? for a pressure of 760 mm Hg ) 04 0002 0002 To pass the test C D c F
6 of IS : 82-1973* Method B in P : 18 (1967) of IS : 1448f with the therm o meter conforming to the requirements given in Appcndix B of this standard IS
Water content, percent by mass, Max Residue on evaporation, g/100 ml, Max Acidity (as CHsCOOH), g/l00 ml, Max Alkalinity Permanganate minute, Min Alcoholic impurities test,
: 2362-19735 : 82-1973 -
8 of IS
*Methods of sampling and test for thinners and solvents for paints (,fird rrzisim ). tIncase the barometric pressure, p, deviates from 7130 mm Hg, USI the correction 0,037 ( p - 760 )C for distillation temperature. IMethods of test for petroleum and its products : P : 18 Distillation (Jrsr r&ion ). Determination of water by the Karl Fischer method (Jrst rerision ).
IS : 170 - 1986 3.22 3.3 The product may also be marked with Standard The use of the Standard
of Indian Standards
mark.
Bureau
Mark is governed by the provisions of the and the Rules and Regulations made t!rereunder. The details of conditions under which the licence for the use of Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards.
Act, 1986
4. SAMPLING
representative
samples
shall be as prescribed
4.2.1 Individual Sam/h - Tests for distillation range and any other characteristic, if so agreed to between the parties, shall be carried out individually on each of the test samples in a set as prepared in G-4.1.
4.2.2 Composite Samples - Tests for determination of remaining characteristics of this standard shall be carried out on the composite sample as prepared in G-4.2. 4.3 Criteria for Conformity
4.3.1 For Composite Samples - The lot shall be declared as conforming to the requirements ofthis standard if each of the test results on the composite sample according to 4.2.2 satisfies the corresponding requirements of this standard. 4.3.2 For Individual Samples - For each of the characteristics tested on the individual samples accordin, u to 4.2.1, the mean and the range of test results shall be calculated as below: Mean, X = sum of test results divided by number of test results SO added; and and minimum values of Range, R = difference between maximum test results. The expressions ( z - 0.6 R ) and ( R + 0.6 R ) shall then be calculated. The lot shall be considered to conform inrespect of the relevant characteristics if ( k + 0.6 R ) is less than the maximum specified value and ( 2 - 0.6 R ) is greater than the minimum specified value.
When the sample size is ten, the test results shall be grouped into two, each constituting five tests results, taking them consecutively in the same order as ob_tained. For each group, the range shall be calculated and the mean range R shall be calculated by dividing the sum of the ranges by two. In the expression ( X f 0.6 R ), R shall be replaced by &?. 6
of Reagents
water
- Unless specified otherwise, pure chemicals ) shall be employed in tests. ( see IS : 1070-1977*
impurities
NOTE - Pure chemicals shall mean chemicals that do not contain which affect the results of analysis.
DETERMINATION
A-1.0 Outlineof
the Method - The colour of the material is compared with that of the colour standard and is expressed in terms of Hazen colour units. The Hazen unit is defined as the colour of an aqueous solution containing 1 ppm of platinum in the form of chloroplatinic acid and 2 ppm of cobaltous chloride hexahydrate ( CoC12*6H20 ), A-l.1 Apparatus
_Nessler Cylinders two, loo-ml Flasks capacity 250 and ( see IS : 4161-1967t 500-ml capacities ). (see
A-l;l;l
Graduated
Hydrochloric Acid -
relative
density
).
A-1.2.3 Chloroplatinic Acid - Dissolve 250 mg of platinum in a small quantity of aqua regia contained in a glass or porcelain basin by heating on a water bath. When the metal has dissolved, evaporate the solution to dryness. Add 1 ml of hydrochloric acid and again evaporate to dryness. Repeat this operation twice more. *Specification for water for general laboratory use ( second rmision ). tSpecification for Nessler cylinders. ISpecification for one-mark volumetric flasks (jirsf revision ). Specilication for hydrochloric acid ( second revision).
IS: 170 .1986 A-l.3 Preparation of Colour Standards - Dissolve 0.50 g of cobaltous hexahydrate and whole of the chloroplatinic acid ( see A-1.2.3 ) of hydrochloric acid. Warm, if necessary, to obtain a clear soluafter cooling, pour into the 500-ml graduated flask. Dilute with the mark and mix well. This solution has a colour of 500 Hazen
A-1.3.1 Pipette 5 ml of this solution ( see A-l.3 ) into a 250-ml graduated flask. Dilute with water up to the graduation mark. This dilute solution has a colour of 10 Hazen units and should always be freshly prepared.
A-l.4 Procedure - Fill one of the Nessler cylinders to the mark with the material to be tested and the other with the colour standard. Using a white background, compare the colours.
FOR THE
THERMOMETER
a) b) Immersion C) Graduations:
1) Subdivisions 2) Long lines at each 3) Number at each
Range
48 to 102%
100 mm
0~2C 1C
2C 0.2OC 395 & 5 mm
4 e) id h)
Max of stem
f-1Outer
diameter
diameter
location
1) Bottom
2)
Specification
for
liquid-in-glass
solid
stem
IS : 170 - 1986 B-1.1.1 Any other thermometer also be used. of similar range and accuracy may
APPENDIX [ Tuble 1,
TEST C-l. REAGENTS FOR
Item (vi) ]
ACIDITY
C-l.1 Pbcnolphthalcin Indicator - prepared by dissolving phenolphthalein in 100 ml of 60 percent ethyl alcohol. C-l.2 Standard Sodium Hydroxide Solution 0.01 N.
0.1 g of
C-2. PROCEDURE C-2.1 Fill 100 ml of water and put a few pieces of clean porous pracelain in a 500-ml conical flask ( non-alkaline glass ) and boil gently for 5 minutes to eliminate carbon dioxide. Cool slightly and add 100 ml of the material. Boil gently for a further period of 5 minutes. At the end of this period, close the neck of the flask with a stopper carrying a sodalime tube, and allow to cool. When cool, remove the stopper, add 0.5 ml of phenolphthalein indicator and examine for alkalinity; if not alkaline, titrate with standard sodium hydroxide solution using a microburette. C-3. CALCULATION C3.t Calculate as follows : Acidity ( as CHsCOOH where ), percent by mass 6 Vfl = -100 D
IS : 170 - 1986
APPENDIX
approximately 0.02 N.
-
D-l.2 D-l.3
Hydroxide
Solution
approximately 0.02 N.
Bromothymol Blue Indicator Solution - prepared by dissolving 0.1 g of bromothymol blue in 100 ml of 50 percent rectified spirit ( see IS : 2263-1979* ). PROCEDURE
D-2.
D-2.1 Take 200 ml of freshly boiled and cooled distilled water in a 500ml conical flask ( non-alkaline glass ). Add 2 drops ( approximately 0.1 ml ) of bromothymol blue indicator solution. Adjust to the neutral colour of the indicator by adding hydrochloric acid or sodium hydroxide solution as necessary. Transfer 100 ml of the neutralized water to each of two 250-ml cylinders. To one of these, add 100 ml of the sample and shake well. Compare the colour ofthe sample with that of the blank, viewing both downwards to compensate for dilution. D-2.2 The material shall be considered change of colour towards blue, indicating place. to have passed the test the presence of alkalinity, if no takes
APPENDIX
TEST
in acetone
which
10
-1986
E-2.1 Substances reacting with potassium permanganate in neutral solutions reduce it to manganese dioxide which colours the solution yellow. In the permanganate test, the time required for the colour of the test solution to change to that of a standard solution is measured. The colour of the test solution changes from pink-orange to yellow-orange. E-3. E-3.1 tubes, APPARATUS Colour Comparison provided with ground Tubes - matched-50 ml, tall form or optically clear glass caps. Nessler
E-3.2 Constant Temperature Bath - capable of maintaining a temperature of 27.0 * 0*5C. It is important that the constant temperature bath be protected from direct light. If a glass constant temperature bath is employed, it should be wrapped or coated with an opaque material. E-3.3 E-3.4 terval E-4. E-4.0 Pipette capable of delivering 2.0 ml of solution. in-
Interval Timer and Clock - capable of measuring a time of 120 minutes or more. A n a 1arm arrangement is desirable. REAGENTS All reagents should be of analytical reagent quality.
E-4.1 Potassium Permanganate Solutiop ( 0.200 g/litre ) - Dissolve 0*200 g of potassium permanganate ( KMn04 ) and dilute to 1 litre with freshly boiled water. Clear glassware is essential for the stability of this solution. The solution should be stored in brown bottles and be prepared fresh every week for use. E-4.2 Uranyl Nitrate Cobaltous Chloride Standard Solution-Weigh O-250 g of cobaltous chloride ( CoCl,*6Hz0 ) and 0.280 g of uranyl nitrate [ UO,( NOs )*, 6Hz0 ] on an analytical balance and dissolve in about 20 ml of water. Transfer to a 50-ml volumetric flask, dilute to the mark and mix thoroughly. E-4.2.1 This standard solution represents the colour of the end point to which the sample solution fades in the potassium permanganate test. This solution is stable and should be kept in a 50-ml glass stoppered Nessler tube which shall be exactly the same as the one in which the test is run. E-5. PROCEDURE
E-5.1 Fill a 50-ml Nessler tube beyond the mark with the sample to be tested and place in a constant temperature bath. Maintain water level in the bath approximately 25 mm below the top of the tube. When the 11
and uermaneanate storaee and handlineP NOTE - Clean the sample _ cvlinders. , equipment with concentrated hydrochloiic acid ( re&ive density I.19 ) to remove residual manganese oxide ( MnOs ) which catalyzes reduction of potassium permanganate. Remove the acid with not less than ten rinsings with distilled water.
E-6.
REPORT
E-6.1 If the residual pink colour of the sample is darker, same or lighter than that of the standard solution, the permanganate time shall be reported as greater than, equal to or less than 30 minutes respectively.
APPENDIX
F-l.1 Agulhons Reagent - Dissolve 0.5 g of potassium bichromate, analytical reagent grade ( conforming to IS : 250-1964* ) in 100 ml of nitric acid ( relative density l-33 ). F-2. PROCEDURE
F-2.1 Take 1 ml of acetone in a test tube. Add 3 ml of Agulhons reagent. Mix and allow to stand at 27 f 1C for 5 minutes. Note if any blue or violet colour, indicating the presence of alcoholic impurities, is produced. F-2.1.1 The material shall be deemed to have passed the test if the test solution shows no blue or violet colouration. --.*Spccitication for potassiu-n bichromate, technical and analytical reagent ( rczised ). 12
IS:170 - 1986
storing and handling G-1.0 In drawing, preparing, following precautions and directions shall be observed.
area
with
good ventilation.
the material being sampled, the sampling instruments for samples shall be protected from adventitious
G-l.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 both, or by rolling, so as to bring all portions into uniform distribution. G-l.5 The samples shall glass containers. be placed in suitable, clean, dry and they air-tight
G-l.6 The sample containers shall be of such a size that but not completely, filled by the sample. G-l.7 Each sample container shall be stopper after filling, and marked with the mark; month and year of manufacture of available ); and other details of sampling, samplers name.
are almost,
sealed air-tight with a suitable manufacturers name or tradethe material; batch number ( if such as the date of sampling and of
G-l.8 Samples shall be stored in such a manner that the temperature the material does not vary unduly from the normal temperature. G-2. G-2.0 SAMPLING The following INSTRUMENTS forms of sampling instrument samples may be used: from various
a) Weighted sampling can for taking in large tanks; and b) Sampling tube. 13
depths
IS : 170 - 1986 G-2.1 Weighted Sampling Can - of suitable capacity, 500 to 1 000 ml and of such a mass as to sink readily in the material to be sampled. It has a long chain or cord attached to permit filling at any desired level ( see Fig.. 1 ). The metal used to weigh the apparatus shall be fitted externally as Irregularities in the metal are likely to contaminate the sample if the mass is fitted internally.
FIG.1
G-2.2 Sampling Tube - It is made of metal or thick glass and is 20 to ~10 mm in diameter and ,100 to 800 mm in, length ( see Fig. 2 ). The upper and lower ends are conical and are 5 to 10 mm in diameter at the narrow ends. Handling is facilitated by two rings at the upper end. For taking a sample, the apparatus is first closed at the top with the thumb or a stopper and lowered until the desired depth is reached. It is then opened for a short while to admit the material and finally closed and withdrawn.
G-2.2.1 For altered slritably. small containers, the size of the sampling tube may be
14
IS : 170 - 1986
*j--5 n
TO 10mm $l
a-20 TO 40 mm fi
-4~5TOlOrnrn
Fxo. 2 G-3.
SAMPLING TUBE
G-3.1
ing to the same ment is known different sizes of and size shall be separate lot.
15
IS I 170 - 1986 G-3.2 For ascertaining the conformity of the material in a lot to the requirements of this standard, tests shall be carried out for each lot separately. For this purpose the number of containers to be selected from a lot shall be as given below: Number of Containers in the Lot Up VN) to 25 100 150 Number of Containers to be Selected (n) 3 4 5 7 10 chosen at random from the lot to The procedure given in IS : 4905SAMPLES
26 ,, 101 ))
151 ,) 300 301 and above G-3.2.1 The containers shall be ensure the randomness in selection. 1968* may be followed. G-4. TEST SAMPLES
AND REFEREE
G-4.1 Preparation of Sets of Samples for Testing Individually Draw with an appropriate sampling instrument ( see G-2 ), material from each freshly opened container and selected as in G-3.2. Keep these representative samples from different containers separately. From each representative sample, draw three equal portions of the material, each sufficient for carrying out the intended tests, and transfer them into thoroughly clean and dry sample containers. Seal the sample containers air-tight. Thus. three sets of test samples are obtained such that each set has a test sample from each selected container. Send one each of these sets to the purchaser and the supplier. Reserve the third set as referee sample bearing the seals of the purchaser and the supplier. Keep the referee sample at a place agreed to between the purchaser and the supplier. G-4.2 Preparation of Composite Samples - Draw with an appropriate sampling instrument ( see G-2 ), equal portions of material from each container selected as in G-3.2, and mix them thoroughly together to constitute a single composite sample. Divide this composite sample into three parts, each sufficient for carrying out the intended tests, and transfer them to thoroughly clean and dry sample containers. Send one each of these to the purchaser and the supplier. Reserve the third composite sample as referee sample bearing the seals of the purchaser and the supplier. Keep the referee sample at a place agreed to between the purchaser and the supplier.
*Methods for random sampling.
16
BUREAU
OF INDIAN
STANDARDS
Headquarters: Manak Bhavan. 9 Bahadur Shah Zafar Marg. NEW DELHI 110002 Telephones: 323 0131, 323 3375. 323 9402 Fax : 91 11 3234062, 91 113239399, 91 113239382 Telegrams : Manaksanstha (Common to all Offices) Central Laboratory: Plot No. 20/9. Site IV, Sahibabad Regional Central Eastern Northern Southern Offices: Industrial Area, SAHIBABAD 201010 Telephone 877 00 32
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