1S: 6613 = 1972 Indian Standard SPECIFICATION FOR NEUTRAL SPIRIT FOR ALCOHOLIC DRINKS UDC 661-722 ; 663°5 © Copyright 1972 INDIAN STANDARDS INSTITUTION MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 1 _ November 1972 Bevised PriceIS : 6613 - 1972 Indian Standard SPECIFICATION FOR NEUTRAL SPIRIT FOR ALCOHOLIC DRINKS Alcohols and Allied Products Sectional Committee, CDC 2 Chairman Representing Dr S. M. Sua Polychem Ltd, Bombay Members Sunt R. 8. Kasirvar (Alternate to Dr S. M. Shah) Suet J. Banerjer Union Carbide India Ltd, Caleutta Surr V. N. Kuzare ( Alternate) Suat D. K. Basu The Alkali & Chemical Corporation of India Ltd, Calcutta Dr B.S. Mout ( Alternate ) Sunt H. P. Buacar Carew & Co Ltd, Calcutta Supt S. N. Panpey ( Alternate ) Suet O. P. BuaTta All India Distillers’ Association, New Delhi Suri B. L, Kianna ( Alternate ) Sur A. K. BHATTACHARYYA National Test House, Calcutta Dr D. K. Das ( Alternate ) Sut Buurenpra SixcHt State Trading Corporation of India Ltd, New Delhi Surt N.C. Demsza ( Alternate ) Dr S. Bose National Sugar Institute, Kanpur Suri M. L. Darr Ministry of Defence Suri P.N. Senourra (Alternate ) ‘Suri V. Venucorat Natu ‘The Mysore Acetate & Chemicals Co Ltd, Bangalore Dr B.D. Parex Indian "Chemical Manufacturers Association, Calcutta Sunt M. S. Sastry ( Alternate) ‘Surt V. S. RAMANATHAN Central Revenues Control Laboratory, New Delhi Suet D. K. Sankaran ( Alternate ) Suar T. K, Ranoaswaat B. I. D.— Parry Ltd, Nellikuppam REPRESENTATIVE Government of Uttar Pradesh (Industries Depart- ment ) Dr S. N. Tewarr Directorate of Medical and Health Services, Lucknow Sur J. L, THARKAR Indian Drugs & Pharmaceuticals Ltd, New Delhi Dr K.S. Tiwarr Directorate General of ‘Technical ' Development, jew Delhi Dr K. Kumar ( Alternate ) (Continued on page 2) INDIAN STANDARDS INSTITUTION MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 1IS : 6613 - 1972 ( Continued from page 1) Members Representing SurrD. M, Triveot Synthetics & Chemicals Ltd, Bombay Surr H.C. Cxopra ( Alternate ) Suet T. M. XAviER The Sirsilk Limited, Hyderabad Sunt S. K. RaMAKRISHNAN ( Alternate) Sunt D. Das Gupra, Director General, ISI ( Ex-oficio Member) Director ( Chem J Secretary Suat M. A. U. Kuan Assistant Director (Chem ), IST Panel for Monohydric Alcohols, GDC 2: Pl Convener Dr S. M. Suan Polychem Ltd, Bombay Members Surr R. S. Kasivar ( Alternate to Dr S. M. Shah ) Suet O. P. Buatia Somaiya Organics (India) Ltd, Barabanki Sunt R. K. Rat ( Alternate ) Dr S, P. BHATTACHARYA Directorate General of Technical Development, ‘New Delhi Dr K. S. Tiwarr ( Alternate) Suet H, G. CHorra Synthetics & Chemicals Ltd, Bombay Da D. Cuoupnury Union Carbide India Ltd, Calcutta Da H. C. Bryawar ( Alternate ) Dr 8. K. Darra National Organic Chemical Industries Ltd, Bombay Suet P. CHAwta ( Alternate) REPRESENTATIVE Government of Uttar Pradesh Suet H. A. Suan Daurala Sugar Works, Daurala _ Sunt V. K. Mani ( Alternate) Stint N, IN. SHANBAG Herdillia Chemicals Ltd, Bombay Supt H. A. Vora Vijay Industries, BombayIS : 6613 - 1972 Indian Standard SPECIFICATION FOR NEUTRAL SPIRIT FOR ALCOHOLIC DRINKS 0 FOREWORD 0.1 This Indian Standard was adopted by the Indian Standards Institution on 14 August 1972, after the draft finalized by the Alcohols and Allied Products Sectional Committee had been approved by the Chemical Division Council. 0.2 The neutral spirit for alcoholic drinks, also known as ‘silent spirit’ is the principal raw material for all Indian made foreign liquors (IMFL ), such as gin, vodka, whisky and brandy. The requirements of Grade ‘I rectified spirit covered by IS : 323-1959* are considered to be inferior, thus they fail to qualify for use in the manufacture of alcoholic drinks. A number of Indian Standards for alcoholic drinks have been prepared and their implementation is linked with the specification of the base material, namely, neutral spirit, This standard has been prepared to ensure an optimum quality of spirit for the manufacture or blending of alcoholic drinks, 0.3 For the purpose of deciding whether a particular requirement of this standard is complied with, the final valuc, observed or calculated, express- ing 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 be the same as that of the specified value in this standard. 1, SCOPE 1.1 This standard prescribes the requirements and the methods of sampling and test for neutral spirit intended for use in the manufacture of alcoholic drinks. 2. REQUIREMENTS 2.1 Appearance — The material shall be clear, colourless and free from any suspended matter. *Specification for rectified spirit (revised ). Rules for rounding off numerical values ( revised ). 31S: 6613 - 1972 2.2 Odour — The material shall have only odour of pure ethanol and no other unpleasant secondary odour. 2.3 Taste — The material shall have no unpleasant taste. 2.4 The material shall also comply with the requirements given in Table 1. 2.5 Special Requirements for Neutral Spirit for Vodka Manu- facture — Neutral spirit required for vodka manufacture shall comply with the requirements of ester content, furfural, aldehydes and higher alcohols as prescribed in Table 2. The other requirements being the same as given in 2 and Table 1. 3. PACKING AND MARKING 3.1 Packing 3.1,1 The material shall be packed in such containers as are agreed to between the purchaser and the supplier, subject to the provisions of law in force for the time being. 3.1.2 All containers, in which the material is packed, shall be dry, clean, free from substances soluble in neutral spirit and leak-free. 3.1.3 Necessary safeguards against the risk arising from the storage and handling of large volume of flammable liquids shall be provided, and all due precautions shall be taken at all times to prevent accident by fire or explosion. 3.1.4 Except when they are opened for the purpose of cleaning and ren- dering them free from alcohol vapour, all containers shall be kept securely closed unless they have been thoroughly cleaned and freed from alcohol vapour. “3.2 Marking —-All containers in which the material is stored or transported shall be marked as prescribed by law in force for the time being. 3.2.1 The containers may also be marked with the ISI Certification Mark. Nore — The use of the ISI Certification Mark is governed by the provisions of the Indian Standards Institution ( Certification Marks ) Act, and the Rules and Regulations made thereunder. Presence of this mark on products covered by an Indian Standard conveys the assurance that they have been produced to comply with the requirements of that standard, under a well-defined system of inspection, testing and quality control during production. This system, which is devised and supervised by IST and operated by the producer, has the further safeguard that the products as actually marketed are continuously checked by ISI for conformity to the standard, Details of conditions, under which a licence for the use of the ISI Certification Mark may be granted to manufacturers or processors, may be obtained from the Indian Standards Institution. 4IS : 6613 - 1972 Su No. xii) xiii) xiv) TABLE 1 REQUIREMENTS FOR NEUTRAL SPIRIT FOR ALCOHOLIC DRINKS Cuaractersmic @ Relative density at 15/15°C Ethanol content, percent by volume at 15°6°C Miscibility with water Alkalinity Acidity (as CHyCOOH ), 3/100 ml, Max Residue on_ evaporation, g/100 ml, Max Esters (as CHsCOOG:Hs ), g/100 ml, Max Lead (as Pb), g/100 ml Methyl alcohol content Furfural content Aldehydes ( as CH;CHO ), g/100 ml, Max Permanganate reaction time, min, Min Copper (as Gu ), g/100 mi, Max isopropyl alcohol, and other ketones acetone (Clause 2.4) Menon or Test ———— Ref to Cl No. of IS : 3752-1967" (3) ©) 0-812 45, to 081679 94 to 96 REQUIREMENT Ref to. Appendix Miscible Nil 0-002 Bw oO 0-002 001 H Nil To pass test To pass test 0-004 Se of this - standard 30 B : | of IS: 323+ - | 1959 | | | 1 i 4 00002 = 16 To pass test C of IS: 1049. = 1962t *Methods of test for alcoholic drinks, {Specification for rectified spirit ( revised ). {Specification for alcohol, perfumery grade ( revised). ee ee ee 5IS : 6613 - 1972 TABLE 2 SPECIAL REQUIREMENTS FOR NEUTRAL SPIRIT FOR ‘VODKA MANUFACTURE (Glause 2.5) Su CHARACTERISTIC Requirement Merson or Trst No. Rer To C1 No. or IS : 3752-1967* ) a) @) (3) @) i) Esters (as CHzCOOCH; ), 2/100 ml, Max 0-005 n ii) Higher alcohols (as amyl alcohol), 0-03 121 percent by volume, Max ili) Aldehydes ( as CHyCHO ), g/100 ml, Max 0-002 13 iv) Furfural (expressed in terms of 100 litres Nil M4 of absolute alcohol ) Method of test for alcoholic drinks. 4, SAMPLING 4,1 Representative samples of the material shall be drawn as prescribed in Appendix A of IS; 323-1959*. 5. TEST METHODS 5.1 Tests shall be carried out by the method specified in col 4 and 5 of Table 1 and col 4 of Table 2. 5.2 Quality of Reagents — Unless specified otherwise, pure chemicals and distilled water (see IS: 1070-1960} ) shall be employed in tests. Nore — ‘Pure chemicals’ shall mean chemicals that do not contain impurities which affect the results of analysis. APPENDIX A [ Table 1, Item (xi) ] DETERMINATION OF ALDEHYDE CONTENT A-1. REAGENTS A-1.1 Standard Sodium Thiosulphate Solution (Na,S,O, )— 0-05 N. A-1.2 Iodine Solution — approximately 0:05 N. ‘Specification for rectified spirit (revised). 4 Specification for water, distilled quality (revised). 6IS :6613 - 1972 A-1.3 Sodium Bisulphite Solution (NaHSO,)— approximately 0-05 N. Nore — This solution will not deteriorate if it contains about 10 percent alcohol; it should not be used after one week. A-1.4 Starch Indicator — Mix about 2 g of soluble starch with cold water to a thin paste. Add about 200 ml of boiling water stirring constantly and immediately discontinue heating. Add about 1 ml of mercury, shake, allow the starch to stand over mercury. Nore — Freshly prepared starch indicator shall be used for the test, A-2, PROCEDURE A-2.1 Place 100 ml of the material in a 500-ml flask, add 100 ml of water and excess sodium bisulphite solution (quantity of sodium bisulphite solution depends on the aldehyde contents in the material; in routine work 20 ml sodium bisulphite solution is found quite satisfactory ) and allow it to stand for about 30 min, shaking occasionally. Add excess iodine solution and titrate this excess with standard sodium thiosulphate solution using starch indicator. Run a blank on 100 ml of water using the same quantities of iodine solution and bisulphite solution as were used in the control test. 4-2.2 Calculation Aldehyde content (as CH,CHO ), g/100 ml = 0-022 (V¥—v) where V =volume of standard sodium thiosulphate solution required for titration in control test, v=volume of standard sodium thiosulphate solution required for titration in the blank, and N = normality of sodium thiosulphate. APPENDIX B [ Table 1, Item (xii)] TEST FOR PERMANGANATE REACTION TIME B-1, APPARATUS B-l.l Graduated Measuring Cylinder —stoppered, 100 ml capacity (see IS : 878-1956* ). “Specification for graduated measuring cylinder. 7IS: 6613 - 1972 B-2, REAGENT B-2.1 Standard Potassium Permanganate Solution — 0-01 N (freshly prepared ). B-3. PROCEDURE B-3.1 Clean thoroughly the graduated measuring cylinder first with concentrated hydrochloric acid, then with water and finally with the material to be tested. Place 20 ml of the material in the cylinder, bring the temperature to 15°C by placing the cylinder in cold water, add 1-0 mi of standard permanganate solution by means of a 1-ml pipette noting down, the exact time as soon as addition is over. Mix the contents at once and keep the cylinder at 15 to 16°C and away from bright light. B-3.2 The material shall be taken to have satisfied the test if the pink colour does not disappear up to 30 min.INDIAN STANDARDS ON ALCOHOLS AND ALLIED PRODUCTS Is: 170-1966 Acetone (firs revision ) 229-1972 Ethyl acetate ( second revision ) 230-1972 Normal butyl acetate (second revision ) 231-1957 Amy! acetate 321-1954 Absolute alcohol ( revised ) 822-1952 Power alcohol 323-1959 Rectified spirit ( revised) 324.1959 Ordinary denatured spirit ( revised) 336-1964 Ether ( revised) 360-1964 Amyl alcohol ( revised ) 361-1962 Normal butyl alcohol, technical ( revised ) 367-1954 Wood naphtha as a denaturing mater 587-1967 Methanol ( methyl alcohol ) ( first revis 695+1967 Acetic acid ( first revision ) 1049-1962 Alcohol, perfumery grade ( revised ) 1235-1958 Acetic anhydride 2252-1962 Diacetone alcohol 2302-1962 Tables for alcoholometry 2631-1964 isopropyl alcohol 2632-1964 Crotonaldehyde 2979-1964 Fusel oil 3506-1967 Tables for alcoholometry ( by Pyknometer method ) 4117-1967 Alcohol denaturants 5860-1970 Tables and inter-conversion charts for ethanol-water mixtures 6618-1972 Neutral spirit for alcoholic drinks ee INDIAN STANDARDS INSTITUTION Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 1 ‘Telephone : 2701 31 (20 lines) Branch Offices: “Sadhna’, Nurmohamed Shaikh Marg, Khanpur F Block, Unity Bldg, Narasimharaja Square 534 Sardar Vallabhbhai Patol Road 5 Chowringhee Approach 5-9-201/2-A ( First Floor ), Chirag Ali Lane 17/418 B Sarvodaya Nagar 54 General Pattors Road Telegrams : Manaksanstha Telephone Ahmedabad 1 20391 Bangalore 2 27649 Bombay 7 3569 44 Calcutta 13, 23-08 02 Hyderabad 1 53435 Kanpur 5 8272 Madras 2 87278 Printed at Delhi Pr ters, Delhi 6, India