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IS 4706-1 (1978): Methods of tests for edible starches andstarch products, Part 1: Physical methods [FAD 16:Foodgrains, Starches and Ready to Eat Foods]

IS : 4706 ( Part I ) • 1978( Kellilirnilaci It)'):' )

Indian StandardMETHODS OF TEST FOR

EDIBLE STARCHES AND STARCH PRC)OUCTS

PART I PHYSICAL METHODS

( First Revision )

UDC 664 • 2 : 543. 03

@ L"'opyrlght 1YilJ

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 RAHADUR Sf-lAI~ :I-Af;AR MAR(;

NEW DEl~HI '1()(X)2

Gr3

III t7H ( Part I) • 1171( R••111nned 1995 J

Indian StandardMETHODS OF TEST FOR

EDIBLE STARCHES AND STARCH PRODUCTSPART I PHYSICAL METHODS

( First Revision)Edible Starches and Starch Products Sectional Committee, AFne 33

Ch••r,"OllSHRI D. S. CHADHA

R"','I1I'.1I,Central Committee for Food Standard. ( Mlnutry of

Health and Family Welfar~ ), New Delhi

( CDlIlllIII,d 0,. /HJI' 2 )

M""b"sSMT DEBI MUKJrEBJB:JC ( AI",,,.,, to

Shri D S. Chadha )Da S Boll!: National Sugar Institute, MlDutry. or Agriculture

at Irriganon ( Department of Food), KanpurDa AN. Salv..8TAVA ( Alt,tu" )

SRRI V. P CHADHA. Bharat Starch & Chemical, Limited, New DeIhlSaRI N. D. SIl'GBAL ( Alt,rndt, )

58B1 CBINlTBHAI MANIBBAI All India Starch Manu(acturers' ASSOCiation, BombaySRRI B. K SARDAN -\ ( Alt,rut, )

SHRI0 P DJIA~IJA Export Inspection Council of India, CalcuttaSHRI P K CHATTERJEE ( Alt,,,,.,, )

DR S S GOTHOSKAR Directorate General of Health SerVJC~I, New DelhiSHRI H R S IYENOAR Indian Confecnonerv Manufacturen' AsSOciation,

New DelhiSaru L 1\ ~1 \THUR ( Alternat« )

SHRI R S 1\ ER Indian Chemical Manufacturers' ASSOCiation.Calcutta

SaRI V S K't LX \RNI ( Alltmall )SHRI R V JCNNARltAlt Anil Starch Products Limited, Ahmadabad

SHRI 0 N PARIKH ( Alt,rna', )DR C R KnlsHNAMOORTHY Tapioca Mark~t Expansion Board, Government or

Kerala, Trrv andrumSHRI S. K, LAKSHMINARAYANA Central Food Technologrcal Research Insntute

( CSIR ). MysoreDR H S. R. DI:IIICACRAR ( Alt,rntJl, )

SHItl 8. Mt·KHERJFE Raval,aon Sugar Farm Limited, Ravalgaon~HRI M. R BRALEBAO ( Alurnat» )

Hitl S R PALEKAR Corn Product. Company (Indaa) Private Limited,Bombay

S!IRI ~f G NaaUItAB ( AlI"1Idl. )

C> Copyrl,h' 1978BUREAU OF INDIAN STANDARDS

Thu pubhcanon II protected under the /lIdltm Cop,,"'" A" (XIV of 19~7) andrenrocucuon In whole or In pari by anv mean. except With written permiu10D of thepublisher .hall be deemed to be 10 anfrlnlement or coPyr1lbt under lhe •• id Act.

IS I t706 ( Part I ) • 1978

( Ctmtiftwd from ptJI' 1 )

Quartermalter General's Branch. Army Headquar-ters, New Delhi

BRIO D. s. R~o

M,mbtrs

SBBI S. RAIIA.WAIIYR,p"smting

Directorate General of Technical Development,New Delhi

Technical Standardization Committee ( Foodstuffs)(Ministry of Agriculture & Irrigation),New Delhi

SSBI J. K. JAGTJANI ( ALI,rnal, )SaBI M. G. SATHB Federation of Biscuit Manufacturers of India,

DelhiSBBI R. D. KEBAWALLA ( Alt""tJI, )

DR P. M. SHAB Maize Products, AhmadabadSSRI V. C. PATEL ( All,mat, )

COL R. N. T.lNBJA

LT.COL D. D. VOJIRA ( A/'lmal, )SaRI T. PURlfAJlANDAJI. Director General, lSI ( EX-Dffici. Memb,r )

Deputy Director ( Agri at Food)

S""tdry

KUMAR1 SSASHI DEVASli,tant Director ( Agri & Food ). IS I

2

IS : 4706 ( Part I ) · 1978

CONTENTS

PAGE

DETBR.MINATION OF VISCOSITY BY REDWOOD VISCOMETER

EXAMINATION FOR DIR.T AND OTHER SUSPBNDBD ANDEXTRANEOUS~ATTEa

7.. DETERMINATION OF RODENT EXCRETA

8. TEST FOR GELATINIZATION AND DETERMINATION OPSTARCH IN GaUEL •••

9. DETERMINATION OF COLOUR or GELATINIZED ALKALINBPASTE ••• ••• •••

QUALITY OP REAGENTS

DETEIt.MINATION OF PARTICLE SIZE

7

7

7

4

5

5

5

6

6

8

9

10

10

•••

...

I ••

MICROSCOPIC EXAMINATION

o. FOUWORD1. SCOPE

2.

3.

4.

5.

6.

10. TasT POR GaLLINO POWER

11. DKTElt.YINAT10N or OUT.a RBSIDUAL SXIN

12. DSTl.aMtNATION 01' COLD-WATER. SOLUBLES

AMENDMENT NO. 1 JUNE 1988TO

IS:4706(Part 1)-1978 METHODS OF TEST FOR EDIBLESTARCHES AND STARCH PRODUCTS

PART 1 PHYSICAL METHODS

(First Revision)

(Pags 6~ olauee ~. 3) - Substitute the followingfor the existing clause:

'5.3 Take 50 ml of the paste and measun! its viscosityin seconds, in the Redwood Viscometer No. 1 at 7SoC.'

(ArDC 33)

Reprography Unitt BIS, New Delhi, India.... ,..,

IS I 4706 ( Part I ). 1978

Indian StandardMETHODS OF TEST FOR

EDIBLE STARCHES AND STARCH PRODUCTSPART I PHYSICAL METHODS

(First Revision)

o. FOR E W 0 R 00.1 This Indian Standard ( Part I ) ( First Revision) was adopted by theIndian Standards Institution on 28 June 1978, after the draft finalized bythe Edible Starches and Starch Products Sectional Committee had beenapproved by the Agricultural and Food Products Division Council.

0.2 This standard was first published in 1968 to cover comprehensivelythe method of test for edible starches. This revision has been taken up toup-date this standard by incorporating other methods employed for qualitycharacteristic determination, and by expanding its scope to cover starchproducts as well. It is being published in two parts. This part coversphysical methods; Part II of this standard covers chemical methods.

0.3 It is expected that the adoption of this standard would help in defin-ing the quality of edible starches and starch products in a manner thatwould enable better quality control. Besides, it will help in achievinguniformity in the methods of test of edible starches, thereby facilitatingthe interpretation and comparison of results.

0.4 In the preparation of this standard, due consideration has been givento the existing methods of test followed by the edible starch industry inthe country. However. wherever possible, alignment has also been madewith the standards formulated by the Technical Committee ISO/TC 93Starch ( Including Derivatives and By-Products) of International Organi-zation for Standardization.

0.5 In reporting the result of a teat or anaJysis made in accordance withthi. standard, if the final value, observed or calculated, is to be roundedoR', it ahall be done in accordance with IS: 2·1960- .

• aulea (or rouacUnl oir DLimerical vaJueI ( ',Pis").

100 ( M1 + Ma)=- ,M

100 MIM

IS I 4706 ( Part I ) • 1978

1. SCOPE

1.1 This standard ( Part I ) prescribes the physical methods used for testingedible starches and starch products.

2. Q,UAUTY or REAGENTS2.1 Unless specified otherwise, pure chemicals and distilled water ( setIS : 1070-1977· ) shall be employed in tests.

NOTE - ' Pure chemical. • .hall mean chemicals that do not contain Impuritieswhich affect the results of analysis.

3. DETERMINATION or PARTICLE SIZE:4.1 Sieve. - Make a nest of two sieves, the upper being ISO-micron ISSieve (see IS: 460-1962t ) and the lower 75-micron IS Sieve (s" IS: 460-1962t) with a cover on top of the upper sieve and a receiver below thelower sieve.

3.2 Procedure - Weigh accurately about 100 g of the material into theupper sieve and fit it with the cover. Place the nest of sieves with thereceiver in a suitable mechanical sieve shaker with tapping action andshake for 15 minutes. Stop shaking, remove the nest ofsieves and transferthe residue on each sieve separately to two tared weighing dishes, using abrush, and weigh each dish.

3.3 CalcalatloD ....... Calculate the percentage of the material retained onthe respective sieves as follows:

a) Material retained on 75-micron IS Sieve,percent by mall

where

M 1 - mus in g retained on 75-micron IS sieve,MI - mass in g retained on I50-micron IS sieve. andM :III masl in g taken for the test.

b) Material retained on 150-micron IS Sieve,percent by mall -

where

M. - ~ass in g of the material retained on ISO-micron ISIleve, and

M - mal. in g of the material taken for the test.

1 .Specification for water for general laboratory use ( "cortd rms;on ).tspecification for test .ievel ( "vi"d ).

5

IS I 4706 ( Part I ) • 1978

4. MICROSCOPIC EXAMINATIONIt

4.1 Apparatus

4.1.1 Mi"oscope - with an eye-piece micrometer calibrated with a slidemicrometer and having a magnification of 300 to 500.

4.1.2 Microscop, Slides

t.I.3 Cover Glasses - either circular or square.

4.2 Procedure --- Take about 1 g of the material and transfer it to abeaker containing 50 rnl of water. Stir the contents of the beaker bymeans of a glass rod to break up granules and lumps and immediatelyplace a drop of the suspension on a clean microscope slide using a glasstube drawn at one end to a small orifice. Press the cover glass on thedrop ot the suspension taking care that no air is trapped between the coverglass and the slide. Remove the excels of liquid on the slide by means ofa blotting paper. Examine the slide, so prepared, under the microscopeto determine the nature of the material and compare with the photomi-crograph shown in relevant Indian Standards.

5. DETERMINATION OF VISCOSITY BY REDWOODViSCOMETER

5.1 ,Apparata-

5.1.1 Rldwood Yiscotnlt" No. 1

5.1.2 Wal,,·Bath with tI Th,rmo-R"ulator

5.1.3 Tim,.R"cDrdi", D,llie, - capable of reading correct to 1 second.

5.2 Proeed.are - From the known moisture content of the test samplecalculate the amount of starch which would give 41 of oven-dry sample.Weigh the amount exactly ancJlltranerer it to a 7SG-ml conical flask. Weighthe flask containing the sample on a pan balance. Add about 25 mlofcold water to the Balk and make the .ample into a fine slurl1" Break anylumps or clots with a gla•• rod flattened at the end. Pour sufficient boilinlwater with constant Itirring to avoid lump formation till the total amountotwater added iejult 200 ,. Boil the pastegently under a reflux condenserfor exactly 1 hour and cool it with constant .tirring to 75°C.

5.3 Measure the VilCOlity or the pute in aecond. in the Redwood visco-meter No. 1 at 75·0.

6

IS I 4706 ( Pari I ) • 1971

6. EXAMINATION FOR DIRT AND OTHER SUSPENDED ANDEXTRANEOUS MATrER

6.1 Procedure -- Take about 10 g of the material in a 250-ml beakerand add 100 ml or water. Stir the material with a glass rod to form asuspension and allow it to stand for 2 hours. Examine the supernatantwater, the surface and the bottom of the sediment for dirt or other susp-ended and extraneous matter.

7. DETERMINATION or RODENT EXCRETA7.1 Apparata.

7.1.1 Beaker, Hooked-Lip -- 250 ml capacity.

7.1.2 Buchner-Funnel

7.1.3 Ruled Paper -- 7 em.

1.2 ReageDts

7.2.1 Chioroform

7.2.2 Carbon Tetrachloride

7.3 Procedure - Weigh 50 g of the sample in 250-ml hooked-lip beaker.Add chloroform to within approximately 1 em of top, mix thoroughly andlet it settle for at least 30 minutes, stirring surface layer occasionally.Decant chloroform and the floating tissue on to the Buchner funnel,taking care not to disturb heavy residue at the bottom of the beaker.Before decanting, take care that the floating layer has not become socompact as to render this operation difficult. Add a quantity of carbontetrachloride equal to the quantity of chloroform and tissue left in thebeaker, let it settle again, and decant a~ before. Repeat this process witha mixture of equal parts ofchloroform and carbon tetrachloride until verylittle tissue remains in the beaker. Wash the residue in the beaker ontoa 7 em ruled paper with a stream of chloroform or carbon tetrachlorideand examine microscopically.

8. TEST POR GELATINIZATION AND DETERMINATION OPSTARCH IN GRUEL

8.1 Procedure

8.1.1 Weigh accurately about 10 g of the material in a 20o-ml conicalflask. Add 80 ml of boiling water into the conical flask. Connect it withan upright water-cooled condenser and heat it on a wire gauze using abunsen burner. (I t is essential that the con ten ts of the flask begin to boilwithin 1 minute of adding the boiling water; ) Boil the contents of the

7

III t706 ( Part I ) • 1178

flask~brilkly for exactly 15 minutes, after which remove the flame, discon-nect the flask from the condenser and filter the contents of the flaskthrough 850-micron IS Sieve ( lei IS : 460-1962* ). Collect the gruel in atared porcelain dish. Pla~e the porcelain dish containing the gruel overa boiling water-bath and evaporate the water from it until the residuebecomes quite dry. Remove the dish from the boiling water..bath andplace it in a electric air-oven maintained at 110 ± 2°C overnight. Coolthe dish in a desiccator and weigh. Repeat, heating in the oven at110 ± 2°C, cooling and weighing at half hour intervals till the differencebetween two successive weighing! is less than 1 mg. Note the lowest mase,

8.1.1.1 Examine the cooked globules or pearls on the sieve for theirglobular shape.

8.2 Calcal.tAo.

Quantity of starch passed into the gruel, _ 101tMlexpressed as percentage by mass ofthe material taken for the test

where

M1 - masl in g of the dry residue obtained from the gruel, andM .. mass in g of the material taken for t he test.

9. DETERMINATION or COLOUR OFGELATINIZED ALKALINEPASTE

9.1 Apparata8

9.1.1 Lovibond Ti"tom,t"

9.1.2 Por&,lain Cuu,'I, - 1 em, supplied by the makers with the LovibondTintometer.

9.2 a_.eat9.2.1 Sodium lbdTOxith Solution - approximately O'5 N, prepared from

sodium hydroxide, analytical reagent {s" IS: 376-1976t ).

9.3 Pr~r.tlo. 01 Materi.l - In case of eoane material taalce about100 g ot the material. I n case of chips, finely powder in a clean mortar10 that the whole of it passes through 250-micron IS Sieve (s" IS : 460-1962-). Place this prepared material in a clean and dry stoppered glassbottle.

-Specification for teat sieve. ( "rJ;s,d ).tSpeelficatioD (or lOdiwn hydroxide, analytical rea,eDt (firsl ",ili." ).

8

IS J 4706 ( Part I ) • 1978

"4 Proceclare

9.4.1 Place about 10 g of the prepared material (9.3) ill a clean anddry neutral glass beaker and add to it 95 ml of water. Heat the beakerwith its contents 011 a boiling water-bath for about 15 minutes withcontinuous stirring till the material is gelatinized. Add 5 ml of sodiumhydroxide solution to the gelatinized paste and stir well. Allow the slurryto cool.

9.4.2 Examisalion of Gelaumred Paste - Clean the porcelain cuvette withcarbon tetrachlorrde to remove any Oily or greasy film Oil It and allow itto dry. Fill the cuvette with the gelatinized paste ( set 9.4.1 ) and placeIt III position In the Tintometer kept In the verucal positron, suitable fOImeasuring reflected light. Place along SIde of it such red and/or yellowLovibond filters as are necessary to match the shade of the gelatmizedpaste, observmg the colour of the gelatinized paste and of the combmationof Lovibond filters through the eye piece.

9.5 Report -- Report the colour of the gelatimzed paste In terms ofIjOVIO()lld uruts by summing up individually the values for tile red andvellow I... ovrbond filters as follows:

Colour reading of the gelatinized pasteIn thta porcelain cuvette ont he Loviboud Scale == «R + by

where

aR = tile SUll1 total of t lie various red Lovibond filters usee). andby - the sum total of various yellow Lovibond filters used.

10. TEST FOR GELLING POWER

10.1 Procedure

10.1.1 'V~lljh approximately 4 g of the mater ial in a porcelain dish,A(Jd 50 1111 of cold w.uer and mix. Heat to borlmg over a bunsen IJIJrnCr,,,1111 JJ1g the content- constantlv. 1301IJ))g nrne shall not exceed I m mu teRemove the flame \\ hen the paste becomes n ansparent a nd 1)( v ms tofroth. Cool to room temperature.

10.1.1.1 The material shall be regardt d (0 have satisfied the u quire-meurs (If the test If the paste formed 011 coolmg is too stiff to llow fromrhe dish.

10.1.1.2 The paste fOI mcd 011 cooling shall be smooth, of uniformconsrsteru )' and free from lumps.

II, 4'. (Part 1)-1'7111. DBTBIlMINATION OF OUTER RESIDUAL SKIN

11.1 Proeed.re

11.1.1 Weigh accurately about 50 K of the material and pick out thechips with outer re.idual skin only. Keep them separately and weigh.

11.2 CaICaiatiOD

Material with outer residualakio, percent by mals _ I~M1

where

Ml .. mu. in g of the material with outer residual skin, andM - mus in g of the material taken for the test.

12. DBTERMINATION OF COLD-WATER SOLUBLES

12.1 proced.re

12.1.1 Weigh accurately about 50 B of the telt sample. Shake it with250 ml of water at room temperature for 30 minutes. Filter the starchluspension by discarding the firlt 25 ml of the filtrate. Collect 100 ml ofthe filtrate in a dish and evaporate it to dryness on a steam-bath and drythe residue to constant weight in an air-oven at 100°C for I hour.

NOT. - Wbatman No. 42 filter paper II surtable for thiS tell. If the filtrateappears ml1ky. It should be filtered agaan.

12.2 Cale.latloD

Cold ...water solubles, percent by mass M x 2'5 X 10 000( on dry basis) - M I X ( 100 - X)"

where

M c= mass in g of the residue,M I :&: mass In g of the sample taken, andX - moisture content percent by mass of the sample.

10

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