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है”ह”ह

IS 5719 (2005): Gelatin, Food Grade [FAD 8: Food Additives]

ts 5719:2005

Ju/y 2005

Wl@w7Fm\ 6 ‘f, @E HmTf&

( W5a7y-tfim)

Indian Standard

GELATIN, FOOD GRADE — SPECIFICATION

(First &vision)

ICS 67.220.20

COBIS 2005

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 ‘BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Price Group 4

— —

. .

Food Additives Sectional Committee, FAD 8

FORE WORD

This-Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized bythe Food Additives Sectional Committee had been approved by the Food and Agriculture Division Council.

Gelatin is widely used in the food processing industry as a stabilizer, gelling agent, emulsifying agent and acrystallization inhibitor. It is also permitted as a food additive under the PFA Rules, 1955.

This standard was first published in 1970 to guide the indigenous manufacturers in making their product conformto international specifications. Considerable assistance was derived from the Pharmacopoeia of India, 1966 andthe British Standard on sampling and testing gelatins in the preparation of the stan-dard. This standard is”beingrevised to update and align with the JECFA specification for gelatin specifically with regards to the limits forheavy metal contaminants and methods of test.

h the preparation of this standard, due consideration has been given to the Prevention of Food Adulteration Act,1954 and the Rules, 1955 framed thereunder. Due consideration has also been given to the Standard of Weightsand Measures (Packaged Commodities) Rules, 1977. However, this standard is subject to restrictions imposedunder these, wherever applicable.

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 or analysis, shall be rounded off in accordance with1S2: 1960 ‘Rules for rounding off numerical values (revised)’. The-number of significant places retained in therounded off value should be the same as that of the specified va[ue in this standard.

IS 5719:2005

Indian Standard

GELATIN, FOOD GRADE — SPECIFICATION

(First Revision)

1 SCOPE

This standard prescribes requirements and methods ofsampling and test for gelatin, food grade which is alsoknown as edible gelatin.

2 RE-l?ERENCES

The following standards contain provisions whichthrough reference in this text, constitute provisions ofthis standard. At the time of publication, the editionsindicated were valid. All standards are subject torevision and parties to agreements based on thisstandard are encouraged to investigate the possibilityof applying the most recent editions of the standardsindicated “below:

1sNo.

1!370:19921699:1995

2491:1998

5401(Part 1): 2002

5402:2002

5887(Part 2): 1976

Title

Reagent grade water (third revision)Methods of sampling and test forsynthetic food colours (secondrevision)Food hygiene — General principles— Code of practice (secondrevision)Microbiology — General guidancefor enumeration of coliforms: Part 1Colony count technique (firstrevision)Microbiology — General guidancefor the enumeration of micro-organisms — Colony count techniqueat 30”C (jirst revision)Methods for detection of bacteriaresponsible for food poisoning:Part 2 Isolation, identification andenumeration of staphylococcusaureus and faecal streptococci @rstrevision)

3 DEFINITION

3.1 Gelatin

Gelatin is a protein produced-by partial hydrolysis ofcollagen derived from skin, tendons, ligaments andbones of animals.

4 REQUIREMENTS

4.1 Description

4.1.1 Gelatin shall be in the form of sheets, flakes,shreds or coarse to fine powder, faint yellow or amberin colour, the shade varying in depth according toparticle size.

4.1.2 Itshall have a slight bouillon like odour. It isstable in air when dry, but is susceptible to microbialdecomposition when moist or in solution.

4.2 Identification

4.2.1 So[ubility

Gelatin is practically insoluble in cold water but shallswell -and soften when immersed in it, graduallyabsorbing from 5 to 10 times its own weight of water.It is soluble in hot water; mixture of hot water andglycerin forming a jelly on cooling; and in acetic acid(approximately 5 N).

Gelatin is practically insoluble in alcohol (95 percent),in chloroform, solvent ether and fixed and volatileoils.

4.2.2 Precipitate Formation

To a solution of gelatin (1 in 100) add trinitrophenol TSor a solution of potassium bichromate (1in 15previouslymixed with about one-fourth its volume of dilutehydrochloric acid, a yellow precipitate shall be formed.

To a sohtion of gelatin ( 1 in 100) add mercuric nitratesolution; a white precipitate shall be formed whichdevelops a brick red colour on warming.

4.2.3 Development of Turbidity

To a solution (1 in 5 000) add tannic acid TS; thesolutkm becomes turbid.

4.2.4 When heated with soda lime, ammonia isevolved.

4.3 The product shall also conform to the requirementsgiven in Table 1.

4.4 The product shall be processe~ packed, stored anddistributed under hygienic conditions in licensedpremises (see IS 2491).

5 PACKING, STORAGE AND MARKING

5.1 Packing

The product shall be filled in ghiss containers or anyother containers wjth as little airspace as possible. Thecontainers shall be such as to preclude contaminationof the contents with metals or other impurities.

5.2 Storage

The product shall be stored in a cool and dry place soas to avoid excessive exposure to heat.

.,.

IS 5719:2005

Table 1 Requirements for Gelatin

(Clause 4.3)

Characteristic RequirementSINo.

(1)

i)ii)

iii)

iv)

v)vi)

vii)

viii)

ix)

x)xi)

(2)

Loss on drying, pereent by mass, MuxGel strength

Total ash, pereent by mass, Mux

Sulphur dioxide, mg/kg, Mar

Nitrogen (on dry basis), percent by mass, Min

Arsenic (as As), mg/kg, Max

Lead (as Pb), mglkg, Ma

Heavy metals, mg/kg, Max

Total bacteria coung per g, Mux.Escherk#ria coli, per g, Max

Faecal streptococci enterococci, per g, Mux

(3)

18To PSSS kst

240

151

5

5010000

10100

Method of Test, Ref to-

%nex of ttds Standard IS -

(4)

AB

cDE—

——

(5)

—.———

15 of IS 169915 of IS 1699

16 of IS 1699

IS 5402Is 5401 (Part 1)

1S5887 (Part 2)

5.3 Marking

Each container shall be legibly and indelibly markedwith the following information:

a)

b)

c)

d)

e)

f)

!3)

Name of the material including the words‘Food grade’;

Name and address of the manufacturer;

Batch or code number;

Net content when packed;

Instruction for storage;

Best before date (Month and year to be givenby the manufacturer); and

Any other requirements as given underthe Standards of Weights and Measures(Packaged Commodities) Rules, 1977 andPrevention of Food Adulteration Act, 1954and Rules framed thereunder.

5.3.1 BIS Certljlcation Marking

The product may also be marked with the Standard Mark.

5.3.1.1 The use of the Standard Mark is governed bythe previsions of the Bureau of Indian Standar& Act,1986 and.the Rules and Regulations made thereunder.The details of conditions under which the licencefor the use of Standard Mark may be granted tomanufacturers or producers maybe obtained from theBureau of Indhm Standards.

6 SAMPLING

Representative samples of the material shall be drawnaccording to the method prescribed in 4 of IS 1699.

7 QUALITY OF REAGENTS

Unless specified otherwise, pure chemicals anddistilled water (see IS 1070) shall be employed in tests.

ANNEX A

~Table 1, S1No, (i)]

DETERMINATION OF LOSS ON DRYING

A-1 PROCEDURE

Weigh accurately about 1 g of the material (do notpowder sheet gelatin while preparing the sample)preferably in a stainless steel dish with an aluminumcover. The dish should weigh about 25 g and shouldhave a diameter of about 70 mm and a height of about15 mm. Add 10 ml of water and allow to soak. Heat ona water-bath to form a homogeneous solution andcontinue heating until most of the water has evaporated.Dry for 2 hat 105°C and for firther periods of 30 minuntil two successive weighings do not differ by morethan 1 mg.

A-2 CALCULATION

loo(y-w2)Moisture, percent by mass = w ~

1-

where

W] = mass of the dish with material beforedrying, in g;

W, = mass of the dish with material after drying,in g; and

W = mass of the empty dish, in g.

2

.,.

IS 5719:2005

ANNEX B

[Tabk 1, S1lVo. (ii)]

DETERMINATION OF GEL STRENGTH

B-1 PROC-EDU-RE 12mm and place the tube in an ice-bath, making certain

Weigh accurately about 1 g and place with 99 of water that the top of the solution is below the level of the ice

in a 200 ml flask. Allow to stand for 15 rein; then place and water. Place the bath containing the tube in a

the flask in a water-bath at 60”C, and swirl occasionally refrigerator, and maintain it at about O“Cfor 6 h. When

until solution is complete. Transfer 10 ml of the the tube is removed from the bath and inverted, no

solution to a test-tube having an internal diameter of movement of the gel shall be observed.

ANNEX C

[Table 1, S1 No. (iii)]

DETERMINATION OF TOTAL ASH

C-1 PROCEDURE is not possible to obtain a carbon-free ash in this way,

Take about 2 or 3 g, accurately weighed, of the ground exhaust the charred mass with hot water, collect the

material in a tared platinum or silica dish previously residue on an ashless filter paper, incinerate the residue

ignited and weighed. Scatter the material in a fine even and filter paper, add the filtrate, evaporate to dryness

layer on the bottom of the dish. Incinerate by gradually and ignite -at a low temperature. Calculate the

increasing the heat (about 555°C), not exceeding dull percentage of ash with reference to the air dried

red heat, until free from carbon, cool and weigh. If it material.

ANNEX D

[Table 1, S1No. (iv)]

METHODS FOR DETERMINATION OF SULPHUR DIOXIDE

D-O GENERAL

Two methods are recommended for the determinationof sulphur dioxide, both of which give consistent andaccurate results. The first method is generally adoptedin the food industry for arbitration purposes. Thesecond method is simpler and quicker.

D-1 METHOD 1

D-1. 1 Apparatus

The apparatus is shown diagrammatically in Fig. 1 andcomprises a round-bottom flask of 1500 ml capacity(preferably provided with two necks) fitted with a leadin tube, passing to within 1.3 cm of the bottom of theflask, connected to a supply of carbon dioxide, andwith a reflux condenser. A tube from the upper end ofthe condenser passes to the bottom of a 250 ml conicalflask which acts as a receiver and which is followed

by two Wohler (Peligot) tubes. All connections aremade by means of glass tubing passing through rubberbungs.

D-1.2 Reagents

D-1 .2.1 Hydrogen Peroxide — 3 percent neutralsolution, free ffom sulphate.

D-1.2.2 Barium Chloride — 10 percent solution.

D-1.2.3 Hydrochloric Acid — 2 N solution.

D-1.2.4 Hyakochloric Acid— concentrated, sp gr 1.1.8.

D-1.2.5 Carbon Dioxide

D-1.2.6 Sodium Hydroxide — 0.1 N solution,accurately standardized,

D-1.2.7 Bromophenol Blue Indicator — Dissolve 0.5 gof bromophenol blue in 7.5 ml of 0.1 N sodium

3

. .

IS 5719:2005

—--_—--“‘‘2‘“/=——--

CONDENSER

1500-ml FLASK

—-—- = =-_-———. ——.

\

L- 250-ml RECEIVER

FIG. 1 APPARATUSFORTHEDETERMINATIONOFSULPHURDIOXIDEMETHOD1

hydroxide solution and dilute to 1000 ml with distilledwater.

D-1.3 P[ocedure

Measure 10 ml of the hydrogen peroxide solution intothe conical flask, add the same quantity into the firstWohler tube. In the second tube (which serves as aguard) place 5 ml of a mixture, of equal volumes ofthe hydrogen peroxide and barium chloride solutions,which has been slightly acidified with 2 N hydrochloricacid solution.

Introduce 500 ml of distilled water and 20 ml of theconcentrated hydrochloric acid into the round-bottomed flask and.boil for a short time in a current ofcarbon dioxide. Allow to cool, while continuing theflow of carbon dioxide, and add about 32 g, accuratelyweighed, of the powdered sample to the flask. For thispurpose, momentarily remove the bung through which

the lead-in tube passes. Heat gently until the gelatin isin solution and then boil for 1h, passing a slow currentof carbon dioxide. Just before the end of the distillation,stop the flow of water through the condenser, to allowany sulphur dioxide, which is retained by thecondensed moisture in the tube of the condenser to bedriven over into the receiver, cooling the lattermeanwhile by immersion in a vessel of water. As soonas the exit from the condenser is hot to the touch at thepoint of entry into the receiverj disconnect from thecondenser and wash down into the receiver withdistilled water. Combine ‘the contents of the firstWohler tube with the liquid in the conical flask, andtitrate cold with the sodium hydroxide solution, usingbromophenol blue indicator. The solution in the secondWohler tube should remain perfectly clear. If anyprecipitate of barium sulphate is formed, the test shouldbe repeated with an increased volume of hydrogenperoxide present in the conical flask and first tube.

4

.,.

IS 5719:2005

D-1.4 Calculation

0.32 TSulphur dioxide, percent by mass = ~

where

T = volume of 0.1 N sodium hydroxide solutionrequired, in millilitres and

W = mass of the sample @ken, in g.

Hence, if exactly 32 g of sample are taken and sodiumhydroxide solution is exactly 0.1 N.

1 ml of sodium hydroxide solution= 100 ppm of S02

D-2 METHOD 2

D-2.1 Apparatus

D-2.1.1 Distillation Apparatus (see Fig. 2) — Itcomprises a special round-bottom flask of 500 mlcapacity, with a steam inlet and outlet connectedto double surface condenser (Davies patternor equivalent). The bottom of the condenser isconnected by means of a glass adaptor to a 250 mlconical flask which acts as receiver. All connectionsare made by means of glass tubing passing throughrubber bungs.

D-2.1.2 Burrette — preferably 10 ml, graduatedin-O.05 ml divisions,

D-2.2 Reagents

D-2.2.1 Sulphuric Acid Solution — Dilute 50 ml of

sulphuric acid, sp gr 1.84 to 250 ml with distilledwater.

D-2.2.2 Hydrogen Peroxide — 10 volumes.

D-2.2.3 Sodium Hydroxide Solution — 0.05 N,accurately standardized.

D-2.2.4 Screened Methyl Red fndicator — Dissolve0.05 g of methyl red and 0.033 g of methylene bluein 200 ml of ethanol.

D-2.3 Procedure

Place 75 ml of distilled water in the flask, introduce20 g of powdered gelatin, followed by 25 ml of thesulphuric acidsolution.Connect flask to the condenser.Place 20 ml of the hydrogen peroxide solution,neutralized to the end point of the indicator, in thereceiver and arrange it so that the condenser adaptordips into the liquid. Pass a current of steam for 10 rein,collecting about 100 ml of distillate in this time. Titratethe distillate with the sodium hydroxide solution, usingthe recommended indicator to green end-point. It isadvisable to titrate in daylight.

D-2.4 Calcuhition

0.16TSulphur dioxide, percent by mass = ~

where

T = volume of 0.05 N sodium hydroxidesolution required, in millilitres; and

W = mass of the sample taken, in g.

. .

IS 5719:2005

fl KTSTEAM INLETr —-

11

u

L—u —

SPECIAL - _:-500mlFLASK

fh- VERYu SMALLe DOUBLE FLAME

SURFACE-CONDENSER

-GLASS

\

250-ml

.——-—If—--— \

r== J 1==–=--/’-—--,

RECEIVER

FIG. 2 APPARATUSFORTHEDETERMINATIONOFSULPHURDIOXIDEMETHOD2

6

,.,.

IS 5719:2005

ANNEX E

[Table 1, S1NO.(V)]

DETERMINATION OF NITROGEN

E-1 APPARATUS

E-.1.1 A recommended apparatus, as assembled, isshown in Fig. 3. The assembly consists of a roundbottom flask A of 1000 ml capacity fitted with a rubberstopper through which passes one-end of the connectingbulb tube B. The other end of the bulb tube B is

connected to the condenser C which is attached, bymeans of a rubber tube, to a dip tube D which dipsinto a known quantity of standard sulphuric acidcontained in a beaker E of 250 ml capacity.

E-1.2 Kjeldahl Flask — capacity 500 ml.

E-2 REAGENTS

E-2.1 Anhydrous Sodium Sulphate

E-2.2 Copper Sulphate

E-2.3 Concentrated Sulphuric Acid — s.pgr 1.84.

E-2.4 Sodium Hydroxide Solution — Dissolve about225 g of sodium hydroxide in 500 ml of water.

E-2.5 Standard Sulphuric Acid — 0.1 N.

FIG. 3 APPARATUSFORDETERMINATIONOFNITROGEN

7

. .

Is 5719:2005

E-2.6 Nlethyl Red Indicator Solution—Dissolve1 g of methyl red in 200 ml of rectified spirit(95 percent by volume).

E-2.7 Standard Sodium Hydroxide Solution — 0.1 N.

E-3 PROCEDURE

E-3. 1 Transfer carefully about 0.3 g of the material,accurately weighed, to the Kjeldahl flask, takingprecaution to see that particles of the material do notstick onto the neck of the flask. Add about 10 g ofanhydrous sodium sulphate, about 0.2 to 0.3 g ofcopper sulphate and 20 ml of concentrated sulphuricacid, .Place the flask in an inclined position. Heat belowthe boiling point of the acid until frothing ceases.Increase heat until the acid boils vigorously and digestfor 30 min after the mixture becomes clear and palegreen or colorless. Cool the contents of the flask.Transfer quantitatively to the round bottom flask withwater, the total quantity of water used being about200 ml. Add with shaking a few pieces of pumice stoneto prevent bumping. Add about 50 ml of the sodiumhydroxide solution (which is sufficient to make thesolution alkaline) carefhlly through the side of the flaskso that it does not mix at once with the acid solutionbut forms a layer below the acid contained in thebeaker. Mix the contents of the flask by shaking anddistil until all ammonia has passed over into thestandard sulphuric acid. Shut off the burner andimmediately detach the flask tlom the condenser. Rinse

the condenser thoroughly with water into the beaker.Wash the dip tube carefully so that all traces of thecondensate are transferred to the beaker. When all thewashings have drained into the beaker, add two or threedrops of methyl. red indicator solution and titrate withthe standard, sodium hydroxide solution.

E-3.2 Carry out a blank determination using all regentain the same quantities but without the material to betested.

E-4 CALCULATION

Nitrogen (on dry basis),140(B-A)N

percent by mass= W.(loo --m)

where

B=

A=

N.

w=

~.

volume of the standard sodium hydroxidesolution used to neutralize the acid in theblank determination, in ml;

volume of the standard sodium hydroxidesolution used to neutralize the excess of acidin the test with the material, in ml;

normality of the standard sodium hydroxidesolution;

mass of the material taken for the test, in g;and

moisture, percent by mass, in the material(see A-2).

.,.

$ Bureau of Indian Standards

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This Indian Standard has been developed from Dot: No. FAD 8 (1473).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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