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“Invent a New India Using Knowledge”

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“Step Out From the Old to the New”

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“The Right to Information, The Right to Live”

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“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 9970 (1981): Dicalcium Phosphate, Food Grade [FAD 8:Food Additives]

IS:9970-1981

Indian Standard SPECIFICATION FOR

DICALCIUM PHOSPHATE, FOOD GRADE

Food Additives Sectional Committee, AFDC 19

Chairman Represeniing

DR K. K. G. MENON Hindustan Lever Ltd, Bombay

Members 7 DR M.J. MULKY ( Alternate to

Dr K. K. G. Menon) CHAIRMAN Technical Standardization Committee ( Food-

stuffs ), ( Ministry of Agriculture & Irriga- tion ), New Delhi

SECRETARY ( Alternate ) DIRECTOR Central Food Laboratory, Calcutta DIRECTOR OF LABORATORIES Directorate of Marketing & Inspection ( Ministry

of Agriculture & Irrigation ), Faridabad SHRI K. L. CHATTERJI ( Alternate)

DRUGS COETROLLER ( INDIA ) Ministry of Health & Family Welfare DEPUTY DRUMS CONTROLLER ( INDIA )

( Alternate ) GOVERNMENT ANALYST King Institute, Madras

PUBLIC ANALYST, COIMBATORE ( Alternate )

DR S. GOVINDARAJAN The Federation of Hotel & Restaurants Association of India, New Delhi

&RI B. HANUMANTHA RAU Bush Boake Allen ( India ) Ltd, Madras DR T. S. SANTHANAKRISEAN (Alternate)

SRRI H. R. S. IYENoAR Indian Confectionery Manufacturers’ Association, New Delhi

JOINT COMMISSIONER ( DD ) DEPUTY COMMISSIONER ( DD )

Ministry of Agriculture & Irrigation

( Alternate ) SHRI J. C. KATHRANI Asian Chemical Works, Bombay; and All Indla

Saccharin Manufacturers’ Association,

DR A. G. NAIR-KURADE SHRI P. MANSUKHANI

SHRI G. K. NAIR (Alternate )

Bombay All India Food Preservers’ Association, New Delhi Glaxo Laboratories ( India ) Ltd, Bombay

( Continued on page 2 )

0 Copyright 1982

INDIAN STANDARDS INSTITUTION

This publication is protected under the Indian Copyright 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:9970 - 1981

( Contimccd ffom page 1 )

SHRI S. N. MEHTA SRRI M. V. DESAI ( Alternate)

SRRI V. K. MENON SHRI N. S. MURTY

SHRI V. K. ATRE ( Alternate ) DR K. M. NARAYANAAN

DR M. K. JAIN ( Alternate ) OFFICER-IN-CHARGE ( CFP ) SHRI S. R. PALEI~AR

SRRI J. V. YARDI (Alternate) SHBI S. RAMASWAY

SHRI S. N. PANDEY ( Alternate ) DR L. V. L. SASTRY

DR A. G. MATHEW ( Alternate) SECRETARY

SHRI I. A. SIDDIQIJI DR R. K. SINHA

DR T. V. SUBBAIH

DR R. K. MEHTA ( Alternate ) SRRI S. B. SULE SHRI M. B. TIJRAKHIA

SHRI B. J. NAVLOOR (Alternate) SHRI T. PURNANANDAM,

Director ( Agri St Food )

Representing

Atul Products Ltd, Atul

Amar Dye Chem, Kalyan Hickson & Dadajee Ltd, Bombay

NationiafnaPairy Research Institute ( ICAR ),

Forest Research Institute & Colleges, Dehra Dun Corn Products Co ( India ) Pvt Ltd, Bombay

Directorate General of Technical Development, New Delhi

Central Food Technological Research Institute ( CSIR ), Mysore

Central Committee for Food Standards ( Ministry of Health & Family Welfare ), New Delhi

Directorate of Sugar & Vanaspati, New Delhi All India Institute of Hygiene & Public Health,

Calcutta Indian Chemical Manufacturers’ Association,

Calcutta

Naarden ( India ) Ltd, Bombay Idachem Industries Pvt Ltd, Bombay

Director General, IS1 ( Ex-o&.s Member )

SHRI V. S. MATHUR Deputy Director ( Agri & Food ), IS1

Preservatives, Anti-Oxidants, Emulsifying and Stabilizing Agents Subcommittee, AFDC 19 : 3

ConDencr

DA G. LAIWEXINARAYANA

MdI?fS GOVERNMENT ANALYST SHRI B. HANUMANTHA RAW

DR T. S. S~THAN AKBISHNAN (Alternate )

Regional Research Laboratory (CSIR ), Hyderabad

King Institute, Madras Bush Boake Allen ( India ) Ltd, Madras

( Continued on page 11 )

Is : 9970 - 1981

Indian Standard SPECIFICATION FOR

DICALCIUM PHOSPHATE, FOOD GRADE

0. FOREWORD

0.1 This Indian Standard was adopted by the Indian Standards Institution on 30 October 1981, after the draft finalized by the Food Additives Sectional Committee had been approved by the Agricultural and Food Products Division Council.

0.2 Dicalcium phosphate has been permitted as dough conditioner for manufacture of certain foods. It is also used as nutrient supplement.

0.3 Chemical Characteristics - Its synonyms are calcium hydrogen phosphate, dibasic calcium phosphate. Chemical names are secondary calcium phosphate, calcium hydrogen orthophosphate, calcium hydrogen phosphate.

0.3.1 Chemical formulae are:

Anhydrous - CaHP04

Dihydrate - CaHPOa* 2H,O

0.3.2 Molecular masses are:

Anhydrous - 136.06

Dihydrate - 172.09

0.4 In the preparation of this standard considerable assistance has been derived from:

Specification for identity and purity of some food additives, FAO Nutrition Meeting Report Series NO. 55 B, FAO/WHO, Rome, 1976; and

Food Chemical Codex 1966. Ed. 1, National Academy of Sciences and National Research Council, Washington DC.

0.5 For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test, shall be rounded off in accordace with

3

IS :9970 A981

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 methods of sampling and test for dicalcium phosphate, food grade.

2. TYPES

2.1 The-product shall be of following two types:

a) Anhydrous

b) Dihydrate

3. REQUIREMENTS

3.1 Description - It shall be white crystals or granules, granular powder or powder.

3.2 Identification

3.2.1 Positive Test for Calcium - Dissolve about 0.1 g of the sample by warming with a mixture of 5 ml of dilute hydrochloric acid and 5 ml of water. Add 3.5 ml of ammonia solution dropwise with shaking and then add 5 ml of ammonium oxalate solution. A white precipitate shall form.

3.2.2 Positi’ve Test for Phosphate - To 10 ml of warm solution ( 1 in 100 ) of the sample containing a slight excess of nitric acid, add 10 ml of ammonium molybdate solution. A yellow precipitate shall form.

3.2.3 Positive Test for Orthophosphate - Wet the sample with silver nitrate solution. A yellow colour shall be produced.

3.2.4 Solubility - The material shall be sparingly soluble in water and insoluble in ethanol.

3.3 The material shall also conform to the requirements given in Table 1.

4. PACKING, STORAGE AND MARKING

4. Packing - The material shall be filled in containers with as little air space as possible. The containers shall be such as to preclude air contamination of the contents with metals or other impurities.

*Rules for rounding off numerical values ( revised).

4

IS : 9970 - 1981

SL N*,.

TABLE 1 REQUIREMENTS FOR DICALClUM PHOSPHATE, FOOD GRADE

( Clause 3.3 )

REQUIRE- METHOD OF TEST, MENT REP TO CL OB

~-___-h~~_~-~ Appendix A IS : 1699-

1974*

(1) (2) (3) (4) (5)

i) Purity as ( CaHPO, ), afrcr drying 98.0 to A-l - at 200°C for 3 h, percent by mass 102.0 A-Z

ii) Loss on drying, percent by mass, after drying at 2CO”C i; ‘r 3h,

a) Anhydrous, Max 2

b) Dihydrate 18 to 22

iii) Fluoride (as F ), mg/kg, Max 50

iv) Lead ( as Pb ), mg/kg, Max 10

v) Arsenic ( as As ), mg/kg, n4a.z 3

vi) Heavy metals ( as Pb ), mg/kg, Max 30

*Method of sampling and test for food colours fjrct r&ion )

- - - -

A-3 -

- 9 - 10

A-4 -

4.2 Storage - The material shall be stored in a cool and dry place.

4.3 Marking - Each container shall be marked legibly and indelibly to give the following information:

a) Name and type of the material including the words ‘Food Grade’;

b) Name and address of the manufacturer;

c) Minimum net mass; and

d) Batch or code number.

4.3.1 The container may also be marked with the IS1 Certification Mark.

NOTE - The use of the IS1 Certification Mark is governed by the provisions of the Indian Standards Institution ( Certification Marks ) Act and the Rules and Rcgula- tions made thereunder. The ISI Mark on products covered by an Indian Standard conveys the assurance that they have been produced to comply with the require- ments of that standard under a well-defined system of inspection, testing and quality control which is devised and supervised by IS1 and operated by the producer. IS1 marked products are also continuously checked by IS1 for conformity to that standard as a further safeguard. Details of conditions under which a licence for the use of the IS1 Certification Mark may be granted to manufacturers or processors, may be obtained from the Indian Standards Institution.

5

IS : 9970 - 1981

5. SAMPLING

5.1 The representative samples of the material shall be drawn according to the method prescribed in Appendix A of IS : 2557-1973*.

6. TESTS

6.1 Tests shall be carried out by the methods specified in co1 4 and 5 of Table 1.

6.2 Quality of Reagents - TJnless specified otherwise pure chemicals and distilled water ( see IS : 1070-19771’ ) shall be employed in tests.

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

APPENDIX A

[Table 1, Item (i) (iii) & (vi)]

METHOD OF TEST FOR DICALCIUM PHOSPHATE

A-O. PURITY

A-0.1 Two methods have been specified. Either could be used depending upon the facilities available.

A-l. METHOD I

A-l.1 Reagents

A-1.1.1 Hydrochloric Acid Solution - 10 percent ( m/v ).

A-1.1.2 Methyl Orange Solution- Dissolve 0.1 g of methyl orange in 100 ml of water and filter, if necessary.

A-1.1.3 Methyl Red Solution - Dissolve 0.1 ml of methyl red in 100 ml of ethanol and filter, if necessary.

A-1.1.4 Ammonium Oxalate Solution - 3.0 percent ( mlv ) in water.

A-1.1.5 Ammonia Solution -Dilute 400 ml of ammonium hydroxide ( 28 percent ) with sufficient water to make 1 000 ml.

A-1.1.6 Dilute Sulphuric Acid - 1 : 6.

A-1.1.7 Potassium Permanganate Solution - 0.1 N.

*Specification for annatto colour for food products. tSpecification for water for general laboratory use (second revision ).

6

IS:9970-1981

A-l.2 Procedure

A-1.2.1 Weigh accurately about 0.3 g of the sample, previously dried for 3 h at 200°C. Dissolve in 10 ml of dilute hydrochloric acid solution, add about 120 ml of water and a few drops of methyl orange solution, and boil for 5 minutes, keeping the volume and pH of the solution in the beaker constant during the boiling period by adding hydrochloric acid or water as necessary. Add 2 drops of methyl red solution, and 30 ml of ammonium oxalate solution. Then add dropwise, with constant stirring, a mixture of equal volumes of ammonia solution and water until the pink colour of the indicator just disappears. Digest on a steam bath for 30 minutes, cool to room temperature, allow the precipitate to settle, and filter the supernatant liquid through an asbestos mat in a Gooch crucible, using gentle suction. Swirl the precipitate in the beaker with about 30 ml of a cold (below 20°C ) wash solution prepared by diluting 10 ml of ammonium oxalate solution to 1 000 ml. Allow the precipitate to settle, and pour off the superna tant liquid through the filter. Repeat this washing by decantation three more times. Using the wash solution, transfer the precipitate as completely as possible to the filter. Finally, wash the beaker and the filter with two IO-ml portions of cold ( below 20°C ) water. Place the Gooch crucible in the beaker, and add 100 ml of water and 50 ml of cold dilute sulphuric acid. Add from a burette 35 ml of 0.1 N potassium permanganate, and stir until the colour disappears. Heat to about 7O”C, and complete the titration with 0.1 .N potassium permanganate. Each ml of 0.1 .iV potassium permanganate is equivalent to 6.803 mg of CaHPO,.

A-2. METHOQ II

A-2.1 Reagents

A-2.1.1 Sodium Hydroxide - Dissolve 4.3 g of sodium hydroxide in water to make 100 ml.

A-2.1.2 Hydroxynephthol Blue Indicator

A-2.1.3 Disodium Ethylenediaminetetra acetate - O-05 m.

A-2.2 Procedure -Weigh accurately about 400 mg of the sample, dissolve in 150 ml of water, and add 15 ml of sodium hydroxide and 300 mg hydroxynaphthol blue indicator. Titrate with disodium ethylendiaminetetra acetate until the solution is clear. Each ml of 0.05 m dissodium ethylenediaminetetra acetate is equivatent to mg of CaHPO,.

A-3. FLUORIDE

A-3.1 Apparatus

A-3.1.1 Assembly as shown in Fig. 1.

7

FIG. APPARATUS FOR LIMIT TEST FOR FLUORIDE

A-3.2 Reagents

A-3.2.1 Pheno?phtkalein Solution - Dissolve 0.2 g of phenolphthalein in 60 ml of 90 percent ethanol and add sufficient water to make 100 ml.

A-3.2.2 Sodium Hydroxide - N.

A-3.2.3 Sulphuric Acid - Concentrated.

A-3.2.4 Sodium Fluoride Solution - containing 50 pg of fluorine.

A-3.2.5 Hydrochloric Acid - 4 JV.

A-3.2.6 <i’ircozium Ali,&n Solution -- Dissolve 0*110 g of zirconium nitrate in water, add a few drops of 4 N nitric acid, and make up to 100 ml with water. Dissolve O-10 g of alizarin sulphonate monohydrate in 20 ml of water, and make up to 100 ml with ethanol. Mix 1 ml of first solution with one ml of the second solution and add 18 ml of water. This solution should be clear and the dilution should be prepared freshly.

A-3.3 Procedure

A-3.3.1 Place about 500 ml of water in flask A (see Fig. 1, ) make it alkaline to phenolphthalein solution with N sodium hydroxide and heat the water to boiling. Leave open the screw clamp at (C).

A-3.3.2 Determine the accurate mass of the sample ( M, in grams ) by the formula M = 50/L, in which L is the fluoride limit, in mg/kg.

IS:9970-1981

Accurately weigh the calculated amount of the sample, place it in flask B, and add 10 ml of water to the flask. Add 17 mlof sulphuric acid slowly down the sides of the flask so that it forms a layer under the water. Connect flask B, to the apparatus. Place the tip of the condenser into a flask containing 5 ml of wat2-r. Mix the contents of flask B, heat to 150°C and slowly shut the screw clamp at C. Regulate the temperature of the solution in the flask B to 150-153% during the distillation. Continue until 170 ml of distillate have been collected.

A-3.3.3 Place the distillate in a loo-ml Nessler tube. Place 80 ml of sodium fluoride solution, containing 50 ug of fluorine, in a second Nessler tube. To each tube add 8.5 ml of 4 N hydrochloric acid and 2.0 ml of zirconium alizarin solution, and make up to 100 ml with water. Let the tubes stand for 15 minutes.

A-3.3.4 The colour of the test solution containing the sample shall not be darker than that of the stac;dard solution.

A-4. HEAVY METALS

A-4.1 Reagents

A-4.1.1 Ammonia Solution-Dilute 400 ml of ammonium hydroxide ( 28 per.:ent ) to 1 000 ml with water.

A-4.1.2 Hydrochloric Acid - 10 percent

A-4.1.3 Lead &bate Stock Solution - Dissolve 159.8 mg of lead nitrate in IO0 ml of water containing one ml of nitric acid. Dilute with water to 1000 ml and mix. Prepare and store the solution in lead-free glass containers.

A-4.1.4 Standard Lead Solution -Dilute 10 ml of lead nitrate stock solution, accurately measured, with water to 100 In!. Each :nl of the solution so prepared contains the equivalent of 10 fig of lead ion (Pb). Prepare the solution on the day of use.

A-4.1.5 Nitric Acid - 10 percent.

A-4.1.6 Sulphuric Acid- 94.5 to 95.5 percent.

A-4.1.7 Acetic Acid - 6 percent.

A-4.1.8 Hydrogen Sulphide - A saturated solution of hydrogen sulphide made by passing H2S in cold water.

A-4.2 Procedure

A-4.2.1 Solution A - Take 2 ml of the standard lead solution in 50 ml Nessier tube and add 23 ml of water. Adjust the flH to between 3.0 to 4.0 by addition of acetic acid or ammonia solution. Dilute with water to 40 ml and mix.

9

IS:9970-1981

A-4.2.2 Solution B - Place 750 mg of the sample, accurately weighed, in a suitable crucible, add sufficient nitric acid to wet the sample, and carefully ignite at a low temperature until thoroughly charred, covering the crucible loosely with a suitable lid during the ignition. After the substance is thoroughly carbonized, add 2 ml of nitric acid and 5 drops of sulphuric acid, and cautiously heat until white fumes are evolved. Then ignite, preferably in a muffle furnace, at 500 to 600°C until the carbon is all burnt off. Cool, add 4 ml of dilute hydrochloric acid, cover and digest on a steam-bath for 10 to 15 minutes. Uncover, and slowly evaporate on a steam-bath to dryness. Moisten the residue with one drop of hydrochloric acid, add 10 ml of hot water, and digest for 2 minutes. Add dropwise ammonia solution until the solution is just alkaline to litmus paper, dilute with water to 25 ml, and adjust the PH to 3-O and 4.0 (PH indicator paper) by the addition of diluted acetic acid. Filter, if necessary, wash the crucible and the filter with 10 ml of water. Transfer to a 50 ml Nessler tube. Dilute the combined filtrate and washing with water to 40 ml and mix.

A-4.2.3 To each tube add 10 ml of freshly prepared hydrogen sulphide, mix and allow to stand for 45 minutes and view down over a white surface. The colour of Solution B shall not be darker than that of Solution A.

10

IS : 9970 - 1981

( Continued from page 2 )

Members Reprcscn t ing

SHRI RAMACHANDRA VIS~ANATE Navasari Oil Products Ltd, Navasari KARNE

SHRI ARV~ND HAN~MANT ~IDWAN~ ( Alternate)

DR S. K. KASHYAP Indian Council of Medical Research, New Delhi DR D. N. ROY ( Alternate)

DR I. M. PATEL Kaira District Cooperative Milk Producers Union Ltd, Anand

DR C. V. RAO (Alternat )

DR R. V. RAO Natiga;lalDairy Research Institute ( ICIR ),

SHRI B. B. SAVDESR PANDE CornBo~;~cts Company ( India) Pvt Ltd,

SRRI S. R. PALE~AR ( Alternate ) DR L. V. L. SASTRY Central Food Technological Research Institute

( CSIR ), Mysore SECRETARY Central Committee for Food Standards ( Ministry

of Health & Family Welfare ), New Delhi SHRI I. A. SIDDIQI Directorate of Sugar & Vanaspati, New Delhi

11

INTERNATIONAL SYSTEM OF UNITS ( SI UNITS)

Base Unite

QUANTITY Length

Mass

Time

Electric current

Thermodynamic temperarurr

L I minors intensrcy

Amount of subsrance

Sopplementary Units

QEASTITY

Plane angle

Solid angle

Derived Units QCANTlTY

Force

Energy

Power

Flux

Flux denslty

Frequency

Elec:ric conductance

Electromotive force

Pressure, stress

UNIT

metre

kilogram

second

ampere

kelvin

candela

mole

UNIT

radian

steradian

UNIT

newton

joule

watr

webcr

tesla

hertz

sicmcns

volt

Pascal

SYMBOL

m

kg

6

A

K

cd

s YXBOL

rad

91

SY.MSOl

N J w Wb

T

H

s v

P.1

DERIN,TI”N

1N = 1 kg.mis2

1J = 1 N.m

IW - lJ/s 1 Wb = 1 V.s

1 T = 1 Wb/m2

1 H = 1 c/s (s-1)

1s = 1 A/V

IV = 1 W/A 1 Pa = I N/m’