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है”ह”ह

IS 2697 (1976): Ammonium bicarbonate for food industry [FAD8: Food Additives]

Gr3 February 1977

Indian Standard *

!S: 2697 - 1976 ( Reafiihncd 1996 )

SPECIFICATION FOP AMMONIUM BICARBONATE FOR FOOD INDUSTRY

( First Revision ) __~ ~~

First Reprint APRIL 1997

UDC 661.523 : 664

0 Copyright 1977

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC

NEW DELHI 110002

lS:2697-1976 ( Reafllnned 1996 )

Indian Stundard

SPECIFICATION FOR AMMONIUM BICARBONATE FOR FOOD INDUSTRY

( First Revision )

Alkalis and Chlorine Sectional Committee, CDC 25

Chairman

SHBI M. L. SEW Members

SIQI A. K. BIIATTAOHAHYYA SEBI A. K. BOSE

SHRI R. C. GIJPTA ( Alternate) SHRI C. A. GHAREKXAN

Representing

Shriram Chemical Industries, New Delhi

National Test House, Calcutta Directorate General of Technical Development,

New Delhi

Calico Chemicals and Plastics Division, T’h+. _Ahmpdabad Mfg & Calico Printing Co Ltd, BornDay

DB A. GUPTA Durgapur Chemicals Ltd, Durgapur SHZI S. K. CHATTERJI ( Alternate )

SHBI L. R. KBISHNAMUBTHY The Mettur Chemical & Industrial Corporation

S,ESI M. PADMANABEAN ( Alternate ) Ltd, Mettur Dam

SHBI M. S. MARBALLI SHRI A. SREEKANTA NAIZ

Tariff Commission., Bombay Tranvancore Cochm Chemicals Ltd, Udyogmandal

SEBI C. N. GOPINATHAN NAIR ( Alternate ) S-1 R. PZABEAKAR Tata Chemicals Ltd, Bombay

SZRI P. V. SUBZAMANYAM (Alternate) REPREBENTATIVE The Travancore Rayons Ltd, Rayonpuram

SERI P. S. HARI’HARKRISHNAN ( Alternate) SHRI B. K. ROY Salt Commissioner, Government of India, Jaipur

SHRI K. K. SAHNI (Alternate) DR A. K. SEN Ministry of Defence ( DGI )

SHRI J. P. AQARWAL (Alternate) DR K. SESHADRI Central Salt & ,Marine Chemicals Researc

Institute ( CSIR), Bhavnagar DR D. R. BAXI (Alternate )

SHRI K. SETH1 IndtiBti;;; St Toiletries Makers’ Association,

SHRI R. S. VAIDYANAT~AN ( Alternate ) ( Continued on Page 2 )

,.. @ Cojyright 1977 .- _.

BUREAU OF INDIAN STANDARDS This publication is protected under the Indim CoPytight Act (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 : 2697 - 1976

( Continued from page 1 ) Members

SHRI D. K. SITARAMAYYA

SHRI JAI G~PAI. JAIN ( Alternate )

SHRI S.P.SIIRIVASTAVA ( Alternate )

SHRI S. SUBBIAH

Reprascnting

Dhrangadhta Chemical Works Ltd, Dhrangadhra; and Indian Chemical Manufacturers’ Associ- ation, Calcutta

Dhrangadhra Chemical Works Ltd, Dhrangadhra

Indian Chemical Manufacturers’ Association, Bombay

Directorate General of Supplies & Disposals, New Delhi

SERI N.G. S. DYER (Alternate) SHRI M. S. TYA~I Indian Paper Makers’ Association, Calcutta SHRI B. R. WALAVAL~AR Saurashtra Chemicals Ltd, Porbandar

SIIRI L. K. MALAVIYA ( Allernate ) DR G. M. SAXENA, Director General, ISI ( Ex-o&cio Member )

Director ( Chem ) Secretary

Srrar S. C. KALRA Assistant Director ( Chem ), IS1

Panel for Alkalis and Allied Products, CDC 25 : Pl

Convener

SHRI B. R. WALAVALEAR

Members

Saurashtra Chemicals Ltd, Porbandar

SHRI L. K. MALAVIYA (&err/ale to Shri B. R. Walavalkar )

SHRI P. S. BHATIA The Ballarpur Paper SK Straw Board Mills Ltd,

SERI A. K. BHATTAOHARYYA Yamuna Nagar

National Test House, Calcutta SHRI S. M. MEETA

Saar M. V. DZSAI ( Alfarnofe ) Atul Products Ltda Atul

SHBI R. N. MODY lndi;irnya;p 8s. Toiletries Makers’ Association,

SHRI R. S. VAIDYA~ATHAN ( ANemote ) SHRI S. S. RAJA~ Standard Alkali Chemical8 Divirion, Bombay

SHRI T. P. VEXKATARAMAN (Alternate) SHIU M. R. RAMAOHANDRAI

SHRI N. B. PATEL ( Altcmate ) Tata Chemicals Ltd, Bombay

SHBI P. R. RAYANATHAN Tata Oil Mills Co Ltd, Bombay SHBI RAMESE CHAWD All India Glass Manufacturers’ Federation,

New Delhi SHBI C. K. SOYANY ( Ahmote)

REPREBBINTATIVBI SERI JAI GOPAL JAIN ( Altcrnats)

Dhrangadhra Chemical Works Ltd, Dhrangadhra

Sam P. SESHASAYEEI The Mettur Chemical 8s Industrial Coruoration Ltd, Mettur Dam

SHRI R. V. RAMANI ( Alternate) SHRI M. S. TAWAKLEY Indian Dyestuff Industries Ltd, Bombay

SHRI R. SRINIVASAN ( ~ltctnotr) SHRI S. S. THAKTJR

Sasr P. L. BURMAN ( Alternate) lndian Paper Mills Association, Calcutta

2

IS : 2697 - 1976

Indian Standard SPECIFICATION FO& AMMONIUM

BICARBONATE FOR FOOD INDUSTRY

( First Revision )

0. FOREWORD

0.1 This Indian Standard ( First Revision ) was adopted by the Indian Standards Institution on 2 November 1976, after the draft finalized by the Alkalis and Chlorine Sectional Committee had been approved by the Chemical Division Council.

0.2 This standard was first published in 1964. In this revision more stringent limits for chlorides and copper content have been specified and the methods for determination of ammonium bicarbonate and copper have been modified.

0.3 Ammonium bicarbonate is an important material for the food industry; in particular, the biscuit industry uses it in substantial quantity. This standard is intended to guide the manufacturers and the consumers of this material in producing and selecting, respectively, the material of the right quality.

0.4 For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, express- ing the result of a test or analysis, shall be rounded off in accordance with IS : 2-l 960*. The nuwber 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 ammonium bicarbonate for food industry.

2. REQUIREMENTS

2.1 Description - The material shall be in the form of white crystals or a fine white crystalline powder.

*Rules for rounding off numerical values ( wised ).

3

IS : 2697 - 1976

2.2 The material shall comply with the requirements given in Table 1, when tested according to the methods prescribed in Appendix A. Reference to the relevant clauses of Appendix A is given in co1 4 of the table.

SL No.

CHARACTEBISTIC REQUIREMENT

(1)

i)

(2)

Ammonium bicarbonate, percent by mass, Min

(3)

98.0

METHOD OB TEST ( REF TO CL No. IN

APPENDIX A )

(4)

A-2

ii)

iii)

Chlorides ( as Cl), percent by mass, Max

Sulphates ( as SO, ), percent by mass, Ma.%

0.2

0.1

A-3

A-4

iv)

v)

Iron ( as Fe), percent by mass, Max

Non-volatile matter, percent by mass, Ma.%

0*004

0.1

A-5

A-G

vi) Heavy metals ( as I’o), parts per million, Max

2.5 A-7

vii) Copper ( as Cu ), parts per million, Max 5 A-8

viii) Arsenic ( as As), parts per million, Max 0.6 A-9

ix) Tarry matter To pks test A-10

TABLE 1 REQUIREMENTS FOR AMMONIUM BICARBONATE

FOR FOOD INDUSTRY

3. PACKING AND MARKING

3.1 Packing -The material shall be packed and supplied in polythene- lined steel drums or polythene-lined gunny bags or as agreed to between the purchaser and the supplier.

3.2 Marking - The packages shall be securely closed and marked with the following information:

a) b) c> 4

Name of the manufacturer and his recognised trade-mark, if any; Name of the material;

Mass of the material in the package; and

Lot or batch number in code or otherwise.

4

h : 2697 = 1976

3.3 BIS Certification Marking

The product may also be marked with Standard Mark.

3.3.1 The use of the Standard Mark is governed by the provisions of the Bureau of Indian Standards Act, 1986 and the Rules and Regulations made thereunder. 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.

4. SAMPLING 4.1 Representative samples of the material shall be drawn and their criteria for conformity shall be determined in accordance with the methods prescribed in Appendix B.

APPENDIX A ( Clause 2.2 and Table 1)

ANALYSIS OF AMMONIUM BICARBONATE FOR FOOD INDUSTRY

A-l. QUALITY OF REAGENTS

A-l.1 Unless specified otherwise, pure chemicals and distilled water ( see IS : 1070-1960* ) shall be used in tests.

NOTBI - ‘ Pure chemicals’ shall mean chemicals that do not contain impurities that affect the .results of analysis.

A-2. DETERMINATION OF AMMONIUM BICARBONATE

A-2.1 Reagents

A-2.1.1 Standard Hydrochloric Acid- 1 N and 0’1 N.

A-2.1.2 Methyl Orange Indicator - Dissolve 0.1 g of methyl orange in 100 ml of water.

A-2.1.3 Thymol Blue Indicator - Warm 0’1 g of thymol blue with 4’3 ml of 0’05 N sodium hydroxide solution and 5 ml of rectified spirit until dissolved. Dilute with 20 percent rectified spirit to 250 ml.

A-2.2 Procedure - Weigh accurately 4 g of the material and dissolve it in a 500-ml conical flask with the aid of 100 ml of freshly boiled and cooled __~ .-._ -

*Specification for water, distilled quality ( revised ).

5

b3 t 2697 l 1976

water. Titrate the solution with standard hydrochloric acid ( 1 l\i j in the beginning and with 0’1 N standard hydrochloric acid towards the end using methyl orange indicator or thymol blue indicator. Convert the volume of hydrochloric acid ( 0’1 N ) used into standard hydrochloric acid ( 1 N ).

A-2.3 Calculation

7.9 VJV Ammonium bicarbonate, percent by mass = -----

M

where V = volume in ml of standard hydrochloric acid ( ‘1 N ) required

for titration, jV r= normality of standard hydrochloric acid, and M = mass in. g of the material taken for test.

A-3. DETERMINATION OF CHLORIDES

A-3.1 Reagents

A-3.1.1 Concentrated JVitric Acid - conforming to IS : 264-1968*.

A-3.1.2 Standard Silver Nitrate Solution - 0’1 N.

A-3.1.3 JVitrobenzene A-3.1.4 Standard Ammonium Thiocyanate Solution - 0’1 N.

A-3.1.5 Ferric Ammonium Sul’hate Indicator - approximately 5 percent.

A-3.2 Procedure - Weigh accurately 20 g of the material, dissolve in water and neutralize with concentrated nitric acid and then add about 5 ml in excess. Boil the solution to expel any dissolved carbon dioxide gas, cool and add 10 ml of standard silver nitrate solution. Add 3 ml of nitrobenzene, shake vigorously and titrate with standard ammonium thiocyanate solution using ferric ammonium sulphate indicator.

A-3.3 Calculation

Chlorides ( as Cl ), percent by mass = 3.546 ( 10 JV~ - VJV, )

M where

N1 = normality of standard silver nitrate solution, V = vo!ume in ml of standard ammonium thiocyanate solution

used in the titration,

.jv-t = normality of standard ammonium thiocyanate solution, and

M = mass in g of the material taken for the test.

*Specification for nitric acid ( jirst revision ).

6

IS I 2697 l X976

A-4. DETERMINATlON OF SULPHATES

A-4.1 Procedure - Dissolve about’ 15 g of the material, accurately weigh- ed, in about 100 ml of water. Determine the sulphates present as directed in IS : 2317-1975*.

A-5. TEST FOR IRON

A-5.1 Apparatus

A-5.1.1 .Nessler Cylinders - of 50 ml capacity.

A-5.2 Reagents

A-5.2.1 Concentruted Hydrochloric Acid - conforming to IS : 265-1962t.

A-5.2.2 Ammonium Persulphate

A-5.2.3 Butanolic Potassium Thiocyanate Solution-Dissolve 10 g of potassium thiocyanate in 10 ml of water. Add sufficient n-butanol to make up to 100 ml and shake vigorously until the solution is clear.

A-5.2.4 Dilute Sulbhuric Acid - 10 percent ( v/v ).

A-5.2.5 Standard Iron Solution -Dissolve 0.702 g of ferrous ammonium sulphate [ FeSOd( NH4 ) 2 S04.6Hz 0 ] in 10 ml of dilute sulphuric acid, add 1 g of ammonium persulphate and heat to boiling. Cool and dilute with water to 1 000 ml. Further dilute 10 ml of this solution to 100 ml. One millilitre of the diluted solution is equivalent to 0’01 mg of iron ( as Fe ).

A-5.3 Procedure - Dissolve 1’000 g of the material in 25 ml of water and neutralize with concentrated hydrochloric acid. persulphate and boil to oxidize the iron.

Add 30 mg of ammonium Cool and transfer completely into

a Nessler cylinder. Add 15 ml of butanolic potassium thiocyanate solution and shake vigorously for 30 seconds. Carry out a control test in another Nessler cylinder using 4 ml of standard iron solution and the same quanti- ties of other reagents. Compare the colour in the butanol layers.

A-5.3.1 The limit prescribed in Table 1 shall be taken as not having been exceeded if the intensity of colour produced in the test with material is not greater than that produced in the control test.

~-6. DETERMINATION 0~ k0~-VOLATILE MATTER

A-6.1 Procedure - Weigh accurately about 10 g of the material in a tared porcelain or silica dish. Heat over a strong flame, cool and weigh till consecutive weighings differ by not more than f 1 mg.

*Method for gravimetric determination of sulphates (first revision ). tspecification for hydrochloric acid ( revised ).

7

IS : 2697 - 1976

A-6.2 Calculation

Non-volatile matter, percent by mass = 100 -G B

where

MI = mass in g of the residue, and

,Ma .= mass in g of the material taken for the test.

A-7. TEST FOR HEAVY METALS

A-7.1 Apparatus

A-7.1.1 .hfessler Cylinders - of 50 ml capacity.

A-7.2 Reagents

A-7.2.1 Concentrated Hydrochloric Acid- conforming to IS : 265.1962*.

A-7.2.2 Standard Lead Solution -Dissolve 1’60 g of lead nitrate in water and make up the volume to 1000 ml, Transfer exactly 10 ml of the solution into a volumetric fla.sk and dilute it again with water to 1 000 ml. One millilitre of the diluted solution contains 0’01 mg of lead ( as Pb ), The solution should be prepared freshly.

A-7.2.3 Potassium Cyanide Solution

A-7.2.4 Acetic Acid - approximately 1 N.

A-7.2.5 Hydrogen Sulphide Solution - saturated.

A-7.3 Procedure- Weigh 4’000 g of the material, dissolve in 40 ml of water, add 15 ml of concentrated hydrochloric acid and evaporate to dryness on, a water-bath. Dissolve the residue in water, add 3 ml of acetic acid and a few drops of potassium cyanide solution, Transfer the contents to a Nessler cylinder and dilute to 30 ml with water. Add 1 ml of acetic acid and 10 ml of hydrogen sulphide solution. Carry out a control test in another Nessler cylinder using 1 ml of standard lead solution and the same quantities of other reagents. Dilute the contents of each cylinder to 50 ml and shake well.

A-7.3.1 The limit prescribed in Table 1 shall be taken as not having been exceeded, if the intensity of colour produced with the material is not greater than that produced in the control test.

A-8. TEST FOR COPPER

A-8.1 Apparatus ._~ _.~

*Specification for hydrochloric acid ( rtvistd ).

IS : 2697 - 1976

A-8.1.1 Kessler Cylinders - of 50 ml capacity.

A-8.2 Reagents

A-8.2.1 Concentrated Hydrochloric Acid - conforming to IS : 265-1976*.

A-8.2.2 Concentrated Nitric Acid - conforming to IS : 264-1968t.

A-8.2.3 Citric Acid

~$3.2.4 Dilute Ammonium Hydroxide Solution - approximately 5 N.

A-8.2.5 Sodium Diethyldithiocarbamate Solution - Dissolve 1’0 g of sodium diethyldithiocarbamate in 1 000 ml of copper-free water. Filter and keep in an amber bottle and protect from strong light.

A-8.2.6 Standard Copper Solution - Dissolve 0’392 8 g of copper sulphate pentahydrate ( CuSO~.5H,O ) in water and make up the volume to 1 000 ml. When required for use, pipette 100 ml of the solution into a 1 000 ml flask and dilute up to the mark with water. One millilitre of this solution contains 0’01 mg of copper ( as Cu ).

A-8.3 Procedure -Weigh 10’000 g of the material and dissolve it in about 20 ml of water. Neutralize with concentrated hydrochloric acid and add 4 to 5 drops of concentrated nitric acid. Boil and cool. Add 1 g of citric acid and adjust pH to 9 by adding dilute ammonium hydroxide. Add 10 ml of sodium diethyldithiocarbamate solution. Dilute to the mark and mix well. In the other Nessler cylinder, carry out a control test using 5 ml of standard copper solution in place of the material,

A-8.3.1 The material shall be considered as not having exceeded the limit prescribed in Table 1, if the intensity of the colour produced with the material is not greater than that produced in the’ control test.

A-9. TEST FOR ARSENIC

A-9.1 Preparation of Solution - Dissolve 1’000 g of the material in minimum amount of dilute hydrochloric acid ( approximately 5 N ).

A-9.2 Carry out the test for arsenic with the solution prepared in A-9.1, as directed in IS : 208%1971$, using 0’001 5 mg of arsenic trioxide for comparison standard.

A-10. TEST FOR TARRY MATTER

A-10.1 Reagent

A-10.1.1 Citric Acid

*Specification for hydrochloric acid ( seccond rcoision ). tspecification for nitric mid (Jrst revision ). $Methods for determination of arsenic (Jrsl rcuision ).,

4

ISt2697-1976

A-10.2 Procedure - Mix 5’0 g of the material with 15 ml of water in a dish and add 7 g of citric acid. Stir until all solids have dissolved.

A-10.2.1 The material shall be taken to have passed the test if no tarry odour is observed.

APPENDIX B ( Clause 4.1 )

SAMPLING OF AMMONIUM BICARBONATE FOR FOOD INDUSTRY

B-l. GENERAL REQUIREMENTS OF SAMPLING

B-1.0 In drawing, preparing, storing and handling test samples, the following precautions and directions shall be observed.

B-l.1 Precautions shall be taken to protect the samples, the material being sampled, the sampling instrument and the containers for samples from adventitious contamination.

El.2 To draw a representative sample, the contents of each container selected for sampling shall be mixed as thoroughly as possible by suitable means.

El.3 The samples shall be placed in suitable, clean, dry and air-tight glass or other suitable containers on which the material has no action.

B-l.4 Each sample container shall be sealed air-tight after filling and marked with full details of sampling, the date of sampling and the year of manufacture of the material.

B-l.5 Samples shall not be taken in a place exposed to weather.

B-2. SCALE OF SAMPLING

B-2.1 Lot - All the containers in a single consignment of the material drawn from a single batch of manufacture shall constitute a lot. If a consignment is declared or known to consist of different batches of manu- facture, the containers belonging to the same batch shall be grouped together and each such group shall constitute a separate lot.

B-2.1.1 Samples shall be tested from each lot for ascertaining conformity of the material to the requirements of the specification.

B-2.2 The number of containers (n) to be chosen from a lot shall depend on the size of lot (Jv) and shall be in accordance with co1 1 and 2 of Table 2.

10

TABLE 2 NUMBER OF CONTAINERS TO BE SELECTED

( Clause B-2.2 ) LOT SIZE NIJMBEROFCONTAINEBS

UU TO BESELECTED

(4

(1) (2)

up to 50 51 to 200 : 201 ), 400 5 401 651 7”

B-2.3 These containers shall be selected at random from the lot and, in order to ensure the randomness of selection, random sampling procedures given in IS : 4905-1968* may be followed.

B-3. TEST SAMPLES AND REFEREE SAMPLE

B-3.1 Preparation of Teat Samples

B-3.1.1 Draw with an appropriate sampling instrument a small portion of the material from different parts of each container selected. The total quantity of the material drawn from each container shall be sufficient to conduct the tests for all the characteristics given under 2 and shall not exceed 1 kg.

B-3.1.2 Mix thoroughly all portions of the material drawn from the same container. Out of these portions, a small but equal

i uantity shall be taken

from each selected container and shall be well mixe up together so as to form a composite sample weighing not less than 600 g. This composite sample shall be divided into three equal parts, one for the purchaser, another for the supplier and the third to be used as referee sample.

B-3.1.3 The remaining portion of the material from each container ( after a small quantity needed for the formation of composite sample has been taken ) shall be divided into three equal parts, each part weighmg not less than 100 g. These parts shall be immediately transferred to thoroughly dried bottles which are then sealed air-tight with stop ers and labelled with all the particulars of samphng given under B-1.4. F he material in each such sealed bottle shall constitute an individual test sample. These indivi- dual samples shall be separated into three identical sets of samples in such a way that each set has an individual test sample representing each container selected. One of these three sets shall be sent to the purchaser, another to the supplier and the third shall be used as referee sample.

B-3.2 Referee Sample - The xeferee sample shall consist of a composite sample (see B-3.1.2 ) and’s set of individual samples ( see B-3.1.3 ) marked

‘Mkthods for random sampling.

11

IS:269301976

and shall bear the seals of the purchaser and the supplier. kept at a place agreed to between the purchaser and the

supplier and shall be used in case of dispute between the two.

for this purpose These shall be

B-4. NUMBER OF TESTS

B-4.1 Tests for the determination of ammonium bicarbonate, heavy metals and arsenic shall be conducted on each of the individual samples.

B-4.2 Tests for the remaining characteristics shall be conducted on the composite sample.

B-5. CRITERIA FOR CONFORMITY

B-5.1 For Individual Samples

B-5.1.1 For Ammonium Bicarbonate - From the test results for ammonium bicarbonate, the mean (X) and the range (R) of the test results shall be calculated ( range being defined as the difference between the maximum and the minimum values of the test results ). The lot shall be deciared to have satisfied the requirement for this characteristic, if the value of the expression ( X - 0’6 R ) is greater than or equal to 98’0.

B-5.1.2 For Heavy Metals and Arsenic- The lot shall be declared as conforming to the requirements for these characteristics, if each of individual samples satisfies the test laid down in A-7 and A-9.

B-5.2 For Composite Samples - The test results on the composite sample shall meet the corresponding requirements specified.

12

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222 39 71

Printed at Pintograph, New Delhi (INDIA).

AMENDMENT NO. 1 APRIL 1986

TO

IS:2697-1976 SPECIFICATION FOR AMMONIUM BICARBONATE FOR FOOD NDUSTRY

(First Revisionl

ktzge 4, Table I, SZ lib.(C), cot 31 - Substitute 'O.lyor '0.2'.

(CDC 56)

Printed at Pnntograph, New Delhi, Ph 5726847