is 10634 (1986): bakery shortening - public.resource.org · amend no.1 to is 10634: 1986 f·1.1.3.1...

36
Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. इंटरनेट मानक !ान $ एक न’ भारत का +नम-णSatyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” प0रा1 को छोड न’ 5 तरफJawaharlal Nehru “Step Out From the Old to the New” जान1 का अ+धकार, जी1 का अ+धकारMazdoor Kisan Shakti Sangathan “The Right to Information, The Right to Live” !ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह Bharthari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 10634 (1986): Bakery Shortening [FAD 13: Oils and Oilseeds]

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Page 1: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 10634 (1986): Bakery Shortening [FAD 13: Oils andOilseeds]

Page 2: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,
Page 3: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,
Page 4: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

IS : 10634 -1986(Reaffirmed 2004)

Indian Standard

SPECIFICATION FORBAKERY SHORTENING

( First Revision)

Second Reprint O("TOBER 2008(Including Amendment No.1)

© Copyright) 986

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 B~HADUR SI1AH ZAFAR MARG

NEW DELHI 110002

Gr 7 + Gr I December 1986

Page 5: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

II I 10634 • 1_

Indian StandardSPECIFICATION FOR

BAKERY SHORTENING

( First Revision)

Oils and Oilseeds Sectional Committee, CAFDC 5

Cui,,,..,.PROF M. M. CHAKRABARTY

R,p"s,nl;ngOil Technologist.' Association of India, Kanpur

MIm6"sPnoJ' A. C. GOPTA (Al',rna', to

Pro! M. M. Chakrabarty)Sa.1 T. N. AOOARWAL Shriram Foods and Fertilizer Industrios, New

Df'lhi

Commission,IndustriesKhadi and VillageBombay

SHRI A. K. RAO (AlI,ma', )SHBIJ. ~. ARHTAPUTllB Ministry of Defence (I)GI )

SHRI~N.AoABWAL(AhnMh)

ASSISTANT DJREOTO't GENBRAL C()Dtral Committe« for Food Standards ( CCFS )(PFA) (~finistrv of Health and Family Welfare),

Nt.·w DelluASIIS"fAN'Jl SBCRBTARY (PFA) ( Al',rnale)

DR B. P. BALIOA Tata Oal Mills Company Ltd. BombayDR N. L. MURTY (AI",,..,,)

nl" N. V. BRINOI Hindustan Lever Limited, BombayDR V. V. S. MAN! ( All,rNa',)

SHRI P. K. CHAKRABARTY National Test House, CalcuttaDU\ROT01\ Central Food Laboratory t Calcutta

SItRI A. K. DHAIt. (.41'""a',)SRal P. V. GUJ'ARATHI

SaRI V. K. B. NAIR (AI,,,,..,,)SHRI R. C. GUPTA Direcrcrat.. Gent'ral of Tcchnicnl Development,

Nf"W DelhiSRal S. N. PAICDRY ( Al'"II.',)

SR'RI C. R. Kal.JlM AMOORTllY Swastik Household and Industrial Products Ltd,Bombay

DR G. LAKSBIiINABAYANA Rt'lional Research Laboratory (CSIR ),Hydt·rabad

( C.,,"nutd Oil I'n" 2 )

C CtI/J.1'WIa' 1986BVREAU OF INDIAN Sl"ANllARDS

Tbil publication i. protected under the l"dla1l C'/J.1,i,1l, Ad (XIV of 1957) andreproductiollin whole or ia part by any meanl (·xctopt with writtt·n pf·rmiuion or the

I publiaber .all be deemed to be all infrilllement or coPyrilht under the laid Act.

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IS I 1063.... 1986

Limited.Detergentsand

Central Organization for Oil Industry and Trade,Bombay

SUUl S. N. Au f, n,\VAL i Altemat« )SHKJ V. M. PAl Karnataka Soap.

Bangalore

M,,,,bers

DB B. M. LAL

Repres,ntin,

Indian Agricultural Research Institute ( leAR),New D~lhi

SUBI T. V. MATHEW Central Agrnark Laboratory. NagpurSHRI K. S. KAMATJI ( Alternat,)

SRRI KAMAJ~ KUMA.It MODI

Directorate of Oilsreds Developrnenr, Hvderabad

Director General, lSI (Ex-offitlo Mtmb" )

Central Warehousing CorpOT,ttlon. New Delhi

Direr torate of Vanaspati, Vegetable Oils andFats ( Ministry of Civil Supplies ), New Delhi

Kusum Products Ltd. Rishra

Sliltl R. J. V.·;ItMA ( ..flte,nal,)S JlIU P. 1~. V l'i Jl w AM JJ II A R,\ ~

SJl In 1\.•A Y K It J~It. A ( Alurnat« )SIlIU M. D. W""''''IK

n« H,AJVIH, Sr~(HI ( Alternate )SHltI So\'rlto;u CIIASHEH,

Director ( Chern )

SHIU R. K. SARl>AR ( Alt,rnat, )SURl G. V. StRUH. Solvent Extractors Association of India, Bomhay

SURI L. KIUSJlA~ KUMAn ( Alternate)Du (SllRIMA'l'I) KA'I~LA SOHNI~ Consumer Guidance Socir..ty of India. HombaySUB! G. K. Soon Vanaspati Manufacturers' Association of India,

New DelhiSHR1 M. S. TJlAKU1\ Godrej Soap, Ltd, BombaySHIn S. D. prJllltUM\14A RAO Oil Technological Research Institute, Anantapur

SHin G. AZlr,J~;\(()J)UIN ( Alt,rnal,)Srmr P. D. V ASJlIST Directorate of Marketing and Inspection

( Ministry of Agriculture ), Faridah.sd

DR K. u, PATIL· ( Alt,rnat, )DR R. K. SHAll

Sunl jAf:VI9H RAI ( Altemat« )DR I. A. Sll>UIC.lI

Se,relaT}DIt. R. K. BA.I \3

Assistant Director ( Chern) J IS I

Oils and Fats Subcommittee, CAFDC 5 : 1

COnVfnl'r

DB G. LAKHHMINARAYANA Regional ResearchHyderabad

Laboratory ( CSIR).

M,mb"sA01UCUJ4TQRAL MARXP;1'ING Directorate of Marketing and Inspection

AnVJ8XR. '1'0 THE GOV'~IUliMJtNT ( Ministry of Agriculture), Nagpur011' INUIA

SURI T. V. MAT1U£W (Alt"nat,)SURfJ. A. ASH'r\PU'I'IUl: Ministry of Defence (DCI)

SJIRI P. K. MAJUMDAR (AII~r"at')

( COfl/inu,d ,tI p." 26)

2

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AMENDMENT NO.1 JULY 1994TO

IS 10634 : 1986 SPECIFICATION FOR BAKERYSH'ORTENING

( First Revision)

( Page 4, clause 3.1, line 1 ) - Insert 'of while to pale yellow in colour'before 'clear in appearance'.

(Page S, clause 3.1, line 5 ) - Insert 'rancidity or staleness' before 'foreignodour or taste'.

(Page 5, clause3.4 ) - Substitute tbe following for the existing clause:

'The material shall contain such quantity of refined SCSal11C oil (see IS 547 :1968), which is sufficient to ensure that when the material is mixed with refinedgroundnut oil in the proportion of 20 : 80, the red colour produced by tbeBaudouin test shall not be lighter tban 2 red units in I-em cell on Lovibond scalewhen tested as prescribed in Appendix A.'

(Page 5, clause3.5 ) - Substitute the following for the existing clause:

'The material shall be free from non-edible oils, mineral oil, castor oil andanimal fats when tested by the methods prescribed in Sections 9, 10, 12, 14, 15and 18 of IS 548 (Part 2) : 1976.'

NOTE - Section 18 of IS 548 (Part 2) : 1976 may be used for detecting the presence ofanimal fat in bakery shortening. Section 21 of IS 548 (Part 2) : 1988 shall be used forconfirmatory testing.'

[ Page 6, Table 1, SI No. (iii) J- Substitute the following for tbe existingmatter;

82.0'iii) Unsapeniflable matter,percent by mass,Max (see Note)

NOTE - In caseof bakery shortening where proportion of rice branoil is more than 30 .percent by mass, the unsaponifiable mauer, percent by mass, Ma shall be 2:5 percentprovided the quantity of ricebranoil of such bakeryshortenin& is declatedon the la6eI.'

[ Page 6, Table 1,51No. (vii) ] - Add the following new item:

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

viii) Nickel, ppm, Max 1.5 E

Price Group 1

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Amend ~o.l to IS 10'34 : 198'

[ Page7, clause 5.1(b) ] - Renumber tbe existingas 5.1 (j) and includethefollowing IS 5.1 (h):

"EvelYpickage of bakerysbortening madefrom more tban 30 percentrice branoil shallbear the following label:

This package of bakeryshortening is made from more than 30 percent rice branoilby mass."

( Page25,Appendix F) - Add tbe following newAppendix:

'APPENDIX F

[ Table 1,51No. (viii)andclause 7.1 ]

DETERMINATION OF NICKEL IN BAKERYSHORTENING

F-O Two metbods have been prescribed, tbe colorimetric method and tbe atomicabsorption spectrometric method. The atomic absorption spectrometric methodis tbe reference method.

F-l COLORIMETRIC METHOD

F-l.1 Reagents

F-l.1.1 Concentrated Ammonia

F-l.I.Z Sodium Citrate - 10percent.

F-l.1.3 Dimetllyl Glyoxime - one percentin ethyl alcohol.

F-l.1.4 Chloroform

F-I.l.5 Ammonia (0.5 M)- 1 : 3.

F-I.l.' Ammonia - 1 : 1.

F-I.l.7 Hydrochloric Acid- 0.5 M and 1 N.

F-l.1.8 Sodium Hydroxide - 2 N.

F-t.1.' Potassium Persulphate - 2 percent.

F-l.1.10 StandardNickelSolution

Dissolve 0.447 9 g of nickel sulphate (NiSCi) (6H20) in water or 0.1 g of 99.9percentpure nickel in 10 ml of nitricacid and wben dissolution is complete, boil

2

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Amend No.1 to IS 10634 : 1986

gently to expel oxides of nitrogen and dilute to 1 litre. This solution contains 0.1DIg/InI of nickel and may be further diluted to O.Otlllgllnl, if necessary.

F-I.l.11 Perchloric Acid- 6 percent,

F-l.I.IZ Bromine IValer

F-I.I.13 Nitric Acid - 1 N.

F-l.Z Procedure

F-I.Z.l Preparation of Sample - Representative sample to give a final solutioncontaining greater than 0.05 but less than 10 ug Ni/ml is weighed into a silicadish and heated to flash point using a Bunsen Burner. When the oil catches fire,Bunsen Burner is removed and the oil is allowed to burn in a hood withoutexhaust. After about 30 minutes the flame ceases on its own and a very smallquantity of residue remains. The residue is heated in low Bunsen flame tillsmoke ceases, before keeping the sample in the muffle furnace. Ashing iscompleted in the muftlc furnace maintaining the temperature at 450°C. Ashingwill be complete within 2 hours. Care is needed to take out the sample from themuffle furnace as the ash is very fluffy and quantity is small.

F-I.Z.I.I Dissolve the ash in t N nitric acid by wanning on the water bath andfiller through ashless Whauuan filter paper and make up to suitable VOIUlllC with1 N nitric acid,

F-l.Z.Z Separation of Nickel by Dimethyl Glyoxime-Chloroform Extraction ­To an aliquot containing about 50 to 100 ppm of nickel add 5 ml of 10 percentsodium citrate. Neutralize with concentrated ammonia and add a few drops inexcess V,H greater than 7.5). Add 2 lui of dimethyl glyoximc (or more as maybe required if such ,,"opper or cobalt is present, that is, extra VOIUlllC or 2 1111 foreach 10 mg of copper and 5 lui for each to mg of cobalt), Extract with three 2 to3 1111 portions of chloroform shaking for 30 seconds each time, Shake thecombined chloroform extracts with 0.5 nil of 1:3 (0.5 M) ammonia, Repeat thewash with another portion of ammonia if 111u(.'h copper or cobalt is present.Shake the ammonia washings with 1 or 2 1111 of chloroform and add the latter tothe chloroform extract, Carry out reagent blank using the same quantity ofreagents.

Return the nickel to the ionic 81.. tc by shaking with t\VO 5-1111 portions of 0.5 Mhydrochloric acid, transfer this solution to 8 IOO-lnl volumetric flask and proceedas per calibration.

If_I.Z.3 C%llr Development

3

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Amend No.1 to IS 10634: 1986

F·1.1.3.1 Methodusingpersulphate for oxidation

F·1.2.3.1.1 Calibration - Transfer 1, 2, 4, 6, 8 and 16 ml of standard nickelsolution (1 011 - 0.01 mg Ni) to six IOO-ml volumetric flasks. Add 5 ml of 1 Nhydrochloric acid. Dilute to SO ml and add 1 ml of 10 percent sodium citrate, 3ml of 2 percent potassium persulphate solution, 15 ml of 2 N sodium hydroxidesolution and finally 1 ml of 1 percent ethanolic dimetbyl glyoxime solution.Heat to 60 to 70°C and keep at the temperature for 5 minutes. Cool to roomtemperature and dilute to volume. Measure the absorbance at 465 om. Plot thephotometric readings of the calibration solution against milligrams of nickelpresent in 100 ml solution.

.....1.2.3.t.Z Develop the colour for sample as described under calibration.

....t .2.3.2 Methodusingbrominefor oxidation

F-I.Z.3.Z.1 Calibration - Transfer 1,2,4,6,8 and 10 ml of standard nickelsolution (1 ",I·O,()) mg) In six 100-lnl volumetric flasks, Add 2 nil of perchlorieacid to each flask. Also prepare aseparate reference solution by adding 2 ml ofperchloric acid to a 1OO-Iul volumetric flask. Dilute to 50 ml and addsuccessively (swirling the flasks between additions) 10 ml of sodium citrate, 5lui of brom jnc water and adjust sufficicnt ammonia (1:1) to bleacb the brominecolour. Add 3 ml of ammonia (1 :1) in excess and cool to room temperature,Add 3 ml of dimethyl glyoximc solution, dilute to the mark and mix (the additionof bromine water, ammonia and dimethyl glyoxime should be made withoutinterruption and subsequent photometric measurementshould be made after 10 :t

2 minutes after addition of dimethyl glyoximc), Transfer a suitable quantity ofthe solution to an absorption cell, (·001 and measure the absorbance at 530 nm.Pint the photometric readings of the calibration solution against milligrams ofnickel Jlcr 100 g of solution.

1:-1.2.3.2.Z Develop the colour for sample as described under calibration andread the absorbance against reagent blank.

F-I.2.4 Calculation

Concentration of nickel Measured Dilution factorin sample (pPIU) = concentration x

(from calibration Mass of samplecurve) in g

FeZ A·I'()1\1IC AhSORlt'rlON Sltr4:(~rrR()MErrl{ICME'rHOD

li'-2.1 Reagents

4

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Amend No.1 to IS 10634 : 1986

F-Z.l.1 Stock Nickel Solution - Dissolve 1 g of 99.99 percent nickel in. minimum volume of I ... I HN03 and dilute to one litre with 1 percent nitricacid.

F-Z.l.% Nitric Acid -IN.

F-Z.Z Procedure

F-Z.Z.l Preparation ofSample - Representative sample to give a final solutioncontaining greater than 0.05 but less than 10 ug Ni/ml is weighed into a silicadish and beated to flash point using a Bunsen Burner. When the oil catches fire,Bunsen Burner is removed and the oil is allowed to burn in a hood withoutexhaust. After about 30 minutes tbe flame ceases on its own and a very smallquantity of residue remains. The residue is heated in low Bunsen flame tillsmoke ceases, before keeping tbe sample in the mume furnace. Asbing iscompleted in tbe muffle furnace maintaining the termperature at 450°C. Ashingwill becomplete witbin 2 hours. Care is needed to take out the sample from themuffle furnace as tbe ash is very fluffy and quantity is small.

F-Z.Z.l.l Dissolve the asb in 1 N nitric acid by warming on the water bath andfilter through ashless Whatman filter paper and make up to suitable volume with1 N nitric acid.

F-Z.Z.z Calibration of Atomic Absorption Spectrometer - Calibrate tneinstrument with 0.2, 0.4, 0.8, 1.6, 2.0, 4.0, 8.0 end 10 f.lg/ml standard nickelsolution by setting the wavelength of 232 om using air acetylene flame and INnitric acid as blank. Theabsorbance is plotted against concentrate.

F-Z.Z.3 Measurement - Run the sample solution into the instrument andcalculate tbe concentrationof nickel in the sample.

F-2.Z.4 Calculation

Concentrationof nickel Measuredin sample (ppm) = concentration x

(FAD 44)

s

Dilution factor

-Mass of sample in g

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IS : 10634 • 1'86

Indian StandardSPECIFICATION FOR

BAKERY SHORTENING

( First Revision )

o. FOR E W 0 R D

0.1 This Indian Standard (First Revision) was adopted by the IndianStandards Institution on 31 January 1986, after the draft finalized by theOils and Oilseeds Sectional Committee had been approved by theChemical Division Council and the Agricultural and Food ProductsDivision Council.

0.2 The specifications for bakery shortening have been prescribed underthe Pretention af Food Adulteration (PF:l) Rules, 19j5 and Veget able OilProducts (Standards of Q}lality ) Drder, 1975 ( V<>P ) issued by Ministries ofHealth and Civil Supplies, Government of India, respectively. A needwas, however, felt to formulate an Indian Standard on this subjectincluding its methods of sampling and test which are not included in thePFA Rules or VOP ( Standards of OJiali ')' ) (:o1lIr~1 Order, 1975.

0.3 This specification is primarily based on the requirements prescribedunder PFA Rules and Vegetdble Oil Products i Standards if OJlalil)') Order,1975 8S amended from time to time. However, in line with the presentpractice, requirements for acid value and refractive index have beenspecified and their correspond ing lim its in terrns of free fatty acids( FFA) and butyro refractometer ( B.R.) reading have also been given.

0.4 This Indian Standard was first published in 1983 anti is now beingrevised to incorporate number of modifications, Some of the changesmade in this standard are as follows:

a) The requirement for' using only refined grade of sesame oilconforming to IS : 547-1968* has been deleted;

b) In order not to unduly burden the testing laboratories thenon-edible oils, the test for which should be carried in routinganalysis, have been specified;

c) A range for the melting point requirement instead of an upperlimit only has been stipulated;

.Specification for sesame oil (sIco"d 'tois;,,. ).

3

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IS I 10634 • 1986

d) Requirement for only a positive test for Vitamin A in additionto the requirement for 25 I.U., when packed, has beenprescribed;

e) The capillary slip method for determination of melting pointand Carr Price method for determining positive test for VitaminA have also been included in this revision;

f) The new definition for vanaspdti to bring in line with PFAspecification has been included; and

g) The requirement for antioxidants and synergists and thedescription clause have also been modified.

0.5 For the purpose of deciding whether a particular requirement of thisstandard is complied with, the final value, observed or calculated,expressing the result of a test or analysis, shall be rounded off inaccordance with IS: 2·1960". The number of significant places retainedin the rounded off value should be the same as that of the specified valuein this standard.

1. SCOPE

1.1 This standard prescribes requirements and methods of sampling andtest for bakery shortening.

2. TERMINOLOGY

2.1 Fer the purpose of this standard, the following definitions inaddition to those given in IS : I 1476-1985t shall apply.

2.1.1 Saki'l ShfJrlenin,g - Bakery shortening means lJQnaspati meant foruse as a shortening or leavening agent in the manufacture of bakeryproducts for promoting' the development of the desired cellular structurein the bakery product with an accompanying increase in its tendernessand volume. "

2.1.2 Vanasptu! - Vanaspati means any refined edible vegetable oil oroils subjected to a process of hydrogenation in any form.

NOTE - However, al per VOP, uantJsjJtlti means hydro,enaled oil m~ant Corhuman consumption.

3. REQ,UIREMENTS

3.1 De.crlptioD - The material shall be clear in appearance on meltingand free from sediments, suspended and other foreign matter, separated

*Rulel for roundill' ofTnumerical value. ( "vl-"ll) •tOlollary of terms relating to oils and fats.

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IS I 10634 • 1986

water, added colouring or flavouring substances or any other suchsubstances or any matter deleterious to health. It shall have acharacteristic odour and taste and shall be free from foreign odour andtaste. Antioxidants and .ynergists, as permitted by the competentauthority, may be added to improve its keeping property. It may alsocontain added monoglycerides and diglycerides or any other permittedemulsifying agents, and if aerated, only nitrogen, or air shall be used fortbe purpose and the quantity of such gas incorporated in the productshall not exceed 12 percent by volume.

3.1.1 The clarity of the material shall be judged by the absence ofturbidity after keeping the filtered sample at 50~ C for 24 hours.

3.2 Raw Materials -- Only prescribed vegetable oils and in suchspecified proportions as modified from time to time by the enforcingauthorities shall be used. These oils shall be free from non-edible oilswhen tested as per IS : 548 ( Part 2 )-1976*.

3.3 The material shall be prepared by a process of hydrogenation of onlyprescribed edible vegetable oils and in such specified proportion asmodified from time to time by the enforcing authorities. Only thosechemicals which can be totally removed and shall have no adverse effecton quality of the product, shall be used in the processing.

3.4 The material shall contain not less than 5'0 percent by mass of rawor refined sesame oil (conforming to IS : 5'l7-1968t) but sufficient toensure that when the material is mixed with refined groundnut oil inthe proportion of 20 : 80, the red colour produced by the Baudouin testshall not be lighter than 2 red units in I-ern cell on I..ovibond scale whentested as prescribed in Appendix A.

3.5 The material shall be free from argemore oil, mineral oil, castor oiland animal fat when tested as prescribed in 10, 12, 15 and 18 ofIS : 548 ( Part 2 )-1976*.

3.6 The material shall be manufactured in the pre mises maintained underhygienic conditions (see IS : 2491-1972: ).

3.7 The material shall also conform to the requirements prescribed. inTable 1.

3.8 OptloDal ReqairemeDt - The solid fat index (dilation value) at15°C shall be not more than 1 000 when tested according to the methodgiven in Appendix E.

-Methods of sampling and test for oils and fats: Part 2 Purity tests ( third rtl-uiora).,Specification for sesame oil (sIcond "vision).:Code Cor hygienic conditions Cor food procts.ing units (first rttrision ).

5

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IS I 106M • 1986

TABLE 1 REQ,UIREMENTS FOR BAKERY SHORTENING( Clausu 3.7 lind 7.1 )

SL CHARAOTERIITIC RI:QOIREXENT METHOD OJ' TEIT, RBI' TONo. r- ......

~

Appendix CI No. in IS :548 ( Part 1 ).

1964-

(I) (2) (3) (4) (S)

i) Moisture, percent by maSI, .Va~ 0·25 5

ii) Acid valuef, Mtut 0·5 7

iii) UDlaponifiablEt matter, percent 2·0 8by mall. Max

iv) Melting point, °C, Ma~ 31-41 B

v) Refractive index at GOGe:. Mira 1·450 5 10

vi) Iodine value, Max 75 14

vii) Synthetic vitamin A, expressedin international units ( I. U. ),per gram.

a) Wh.n packed, Min 25 Cb) At retail outlet Sh~11 pass the test D

-Methodl of sampling and telt for oils and fau: Part 1 Sampling, physical andcbemical tests ~ rtvistd ) .

tThe corresponding figure in terms of free fauy acids ( FFA) when expressed asoleic acid shall be maximum 0·25 percent bv mass.

:This corresponds to butyro refractometer ( B.R. ) reading of 37·4.

~. PACKING

4.1 The material shall be packed in suitably sealed packages, as agreedto between the purchaser and the supplier and as netified from time totime by the enforcing authorities.

5. MARKING

5.1 The container shall be marked with the following particulars:

a) X arne of the material;

b) Manufacturer's name and his recognized trade-mark, if any;

c) Net mals in the container;

d) The words • contains 25 I.U. of vitamin A per gram whenpacked ';

e) Name and quantity of emulsifier;

6

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IS I 10634· 1'8'f) Month and year of manufacture;

g) Batch number or lot number in code or otherwise; and

h) Any other marking specified by the statutory authority.

5.1.1 The product may also be marked with Standard Mark.

5.1.2 The use of the Standard Mark is governed by the provisions of the Bureauof Indian Standards Act, J986 and the Rules and Regulations made thereunder.The details of conditions under which the licence for the use of Standard Markmay be granted to manufactures or producers may be obtained from the Bureauof Indian Standards.

5.2 In addition, the following information shall be suitably marked,either printed on the label affixed to the container, or lithographed orstencilled thereon with indelible ink. for example, in a type size of not lessthan 12·5 mm in case of 15 kg tin containers:

'MADE FROM VEGETABLE OILS ONLY'

6. SAMPLING

6.1 Representative samples of the material shall be drawn as prescribedunder 3 of IS : 548 (Part 1 )-1964*.

6.2 Crlterloa for Coaformlty - A lot shall be declared conforming tothe requirements of this standard if the test results on the compositesamples satisfy the requirements prescribed under 3.

7. METHODS OF TESTS

7.1 Testl Ihall be carried out according to the methods prescribed inIS : 548 (Part 1 )-1964*, and IS : 548 (Part 2 )-1976t for the characteris­tics given in Table 1 (set 3.7 ) and Appendices A, B, C, D and E.

I

7.2 Q,aality of Rea.e.ts - Unless specified otherwise, pure chemicalsand distilled water (SII IS : 1070-1977: ) shall be used in the test.

NOTE-' Pure chemicals' shall mean chemicals that do not contain impuritle.which afFect the result of analy.is.

-Method. of lampliD, and teat for oill and Cats: Part 1 Sampling, phy.ical andchemical te.ta t "lJi.s,d ).

tMethod. oC ••mplinl and telt for aU. and Cats: Part 2 Purity teltl (,lai,d "visi.,. ).*SpecificatioD for water Cor Sener.1 laboratory use (",.,.d "vis.,. ).

7

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IS : '10634 • 1986

,\ P PEN D I X A

( Clauses 1.4 al111 7. J )

TEST FOR THE PRESENCE OF SESAME OIL(BAUDOUIN TEST)

A-O. GENERAL

A-O.l Outline of the Method - 'The dvvelopment of a pel manentpink colour with furfural solution in presence of hydrochloric acidindicates the prpsence of sesa me oil.

A-I. REAGENTS

A-t.l Refined Groundnut Oil - (SII' IS: 51-·~-196B* ) showing negativeBaudouin test.

A-l.2 Dilute Hydrochloric Acid -- relative density 1·123.

A-l.3 Concentrated Ilyd,·ochloric Acid - fuming, relative density1-19.

A-l.4 Furfural SolutioD - 2 percent solution of furfural, distilled notearlier than ~?~ hours prior to the test in rectified spirit ( conforming toIS : 323-1 ((>9t). The reagent is stable up to 3 months kept in arefrigerator_

A-2. APPARATUS

A-2.1 LoviboDd Tiatometer

A-2.2 MeasuriDI C)'liader - 25-Inl capacity.

A-3. PROCEDUR~

1\-3.1 Melt the sample of the vegetable oil product. that is, the bakeryshortening, completely and mix it well at a temperature of about 50°C.

A-3.2 Check for the presence of colouring matter which are chromogenicin the presence of hydrochloric acid, by the method given in A-3.2.1and A-3.2.2_

·SpecificatioD Cor groundnut oil (second ""ision).tSpecification Correctified spirit ( "ml,d).

8

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IS I 10634 - 1986

A-3.2.1 Shake 10 ml of the melted bakery shortening with 10 mlconcentrated hydrochloric acid. Note if any red colour develops in theaqueous layer.

A-3.2.2 If a red colour develops in the aqueous layer, shake 20 ml ofthe melted bakery shortening in a separating funnel for half-a-minutewith 15 ml of dilute hydrochloric acid. During the treatment, do notpermit the temperature of the contents of the separating funnel toexceed that temperature necessary to keep the sample in liquid condition.Draw off the red acid layer which collects at the bottom of the funneland repeat the process until no further colourntion takes place.

A-3.3 Dilute 20 ml of the melted bakery shortening, either the originalsample, if no red colour develops on checking as in A-3.2.1, or aftercomplete removal of the hydrochloric acid layer as in A-3.2.2, with80 ml of refined groundnut oil. Take 5 1111 of this mixture in a 25-mlmeasuring cylinder with glass stopper and add 5 ml of concentratedhydrochloric acid. AJd 0·4 011 of the furfural solution, shake vigorouslyfor 2 minutes and allow to stand for 5 minutes, Tr.msfer the contentsof the measuring cylinder to a separating fUOOt"') and decant the acidlayer through a wet filter paper into a I-CIll Lov ibond cell, cleaned withcarbon tetrachloride and dried. Place the cell in povit ion in a LovibondTintomcter and viewing through the eyepiece of the instrument, matchthe colour shade of the filtrate with the appropi iate combination of redand yellow slides. The colour, which is recorded in terms of red unitsonly (correct to one place of decimal ) shall be n-ad within 5 minutes ofthe addition of furfural solution.

A-3.4 Perform a blank experiment using 5 ml of refined groundnut oilin place of the mixture and determine the colour. The Baudouin testreading of the sample shall be the colour reading given by the samplein A-3.3 less that given by the blank.

APPENDIX B

[ Table 1, Item (iv) and Clause 7.1 ]

DETERMINATION OF MELTING POINT OFBAKERY SHORTENING

B-1. APPARATUS

8-1.1 MeitiDI Point Tubes - Thin-walled, uniformly-bored capillaryglass tubes, open at both ends and having the following dimensions:

a) length, 50 to 60 mrn;

9

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IS I I063t • 1986

b) inside diameter, 0-8 to I-I mm; and

c) outside diameter, 1-2 to 1-5 mm,

8-1.2 Thermometer - Centigrade, with 0-20 sub-divisions and a'Suitable range_ The thermometer should be checked against a standardthermometer which has been calibrated and certified by the NationalPhysical Laboratory, New Delhi.

B-l.3 Beaker - with a side-tube heating arrangement.

B-l.4 Water Bath - maintained at 15-17°C.

B-l.5 Heat Source - Gas burner or spirit lamp.

B·2. PROCEDURE

'B-2.1 Melt the sample of the bakery shortening completely and mix it wellat a temperature of about 50°C. Insert the melting point tube ( thoroughlycleaned and dried before use) into the molten product 10 that a columnof the product about 10 mrn long, is forced into it. Allow the sample inthe tube to just set, by keeping the tube in a horizontal position duringwinter; during summer, the tube loay be put on a perforated metal traywhich is so placed inside tho water bath ( at 15-17 tJC) that the bottom ofthe tray just touches the water. Then place the tube in a test-tubeimmersed in water at 15·17 JC~ for one hour. Remove the meltingpoint tube and attach it with a rubber band or any other suitable meansto the thermometer so that the lower end of the melting point tube iseven with the hottom of the bulb of the thermometer. Pour water at about20°C into the beaker (with side-tube heating arrangement) and suspendthe thermometer in the centre of the beaker so that the lower end of thesample column is 30 rom below the surface of water. Heat the side-tubeof the apparatus gently, so that the temperature of water increases slowlyat the rate of 2°0 per minute till the temperature reaches 30°C andthereafter at the rate ofO·S'JC per minute. Note the temperature of thewater when the sample column commences to rise in the tube which isthe melting point of the sample,

APPENDIX C

[ Table 1, Item (vii) and Clause 7.1 ]

DETERMINATION OF VITAMIN A

C-l. GENERAL

C·l~l Priaciple - The content of vitamin A is determined by measure­ment of the ultraviolet absorption spectrum of a fraction, in which the

10

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IS I 10634 - 1986

vitamin A alcohol is collected after its isolation by chromatography. Itis expressed in International Units per gram.

c-l.l.1 One International Unit (I.U.) of vitamin A is equivalent to0·3 ILK vitamin A alcohol or 0·344 Ilg vitamin A acetate.

NOTB - The official method in use in the United Kinldom (UK ). involve. asomewhat differ~nt procedure to that given in this method but both techniques livethe same result for vitamin A.

C-2. REAGENTS

C-2.1 Pota••ium H)'droside - 50 percent aqueous solution.

C-2.2 EthaDol - 96 percent ( t'/v ).

0-2.3 Diethy. Ether - peroxide-free.

NOTE - Make dierhyl ether peroxide-free by distillation over potassiumhydroxide, Store the peroxide-Iree ether over coarse granular carbon.

0-2.4 Petroleum Ether - distilled over potassium hydroxide, boilingrange 40 to 60°0.

C-2.5 AlumiD. (Activated) - Heat the alumina at 6000 C for 6 hours,cool, sieve through a 180 mesh sieve and add about 3 percent water.Mix thoroughly and allow the product to stand for at least 12 hoursbefore use. Store in an air-tight bottle.

C-2.6 AlamiD. (Alk.IIDe) - The lame alumina as given in C-2.5 istreated with sodium hydroxide as follows:

Stir 10 g alumina with a solution of I g sodium hydroxide in 10mlwater. Allow to stand at room temperature for one hour in a closedbottle and shake occasionally. Then heat in a dish in a vacuum dryingoven at IOOcC and 20 mmHg for 2i hours. Pour the dried product intoa bottle without removing any powder clinging to the wa 11 of the dish andstopper securely. To the cooled powder, add 2 percent water and mixthoroughly. Allow to stand for 18 hours and determine the moisturecontent after drying for one hour in a drying oven at 105°C; if lower than~ percent, again add water, mix and repeat the process.

C-2.7 A_llmoD)' Trichloride Solutio. - With a porcelain spoon,introduce 65 g of antimony trichloride into a 500-ml conical flask andwash several times with 15 ml chloroform until the chloroform remainsclear. Then dil.olve the antimony trichloride in 200 ml of chloroformby refluxing. Transfer the warm solution to a bottle containing8nyhydrous sodium sulphate.

II

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IS I 10634 • 1986

NO'l'E - The chloroform to be used should be washed with water and driedbefore use to remove any alcohol which may have been added to improve it. keepingproperties.

After some days antimony trichloride crystals are formed at thebottom and the wall; the solution is then quite clear and ready for use.

C-2.8 Acetone - conforming to IS : '70-1976*.- - - - .- - -. - ~ - ~ .... ~.-. --- .- ..

NITROGENINLET~

200-ml FlAStc

ALKALINEPYROGAllOLSOLUTION

Flo. 1 ApPARATUS POR SAPONIFICATION

0-3. APPARATVa

C-3.1 Comcal FIa.k - 50 mI.

0-3.2 SeparatID.l'aaaeJ. - 500 ml,

·SpecificatioD Coraceto.. ("e,nd ,.uNII).

12

-,

.J

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0-3.3 Rouad Bottom Flask - ~OO ml with ground glass stopper andtwo condensers.

20D--ml FLASK

NITROGENINLET~

ALKALINEPYROGALLOLSOLUTION

---------------- -----,I

It

__ ..J

WATERINLET~

FIG. 2 ApPARATUS FOR EVAPORATION

C-3.4 Chromatographic: Apparatus (Fig. 3 to 6) - The apparatusconsists of two parts, each containing a chromatographic column, whichmay readily be connected in series by means of a rubber stopperconnection. The upper tube contains alumina, the lower alkaline alumina.Close both the tubes at the bottom with a plug of cotton wool. Fill thelonger tubes with petroleum ether to a level which reaches into thewidened section, and then very regularly and gently pour out the alumina.to a column height of 15 em. Fill the shorter column, shortly before use,in the same way to a height of 2 em with alkaline alumina.

C-3.5 Tabes - calibrated at l-ml (see Fig. 5 ).

0-3.6 Pipette -.t-ml with a fine tip.

C-3.7 Gr.d.ated FI••k - IO-ml.

C-3.8 Ultnvlolet Spectrophotometer

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18 I 10634 • 1986

[ PRESSURI!

RELEASE toATMOSPHERe

~PRESSURE

FlO. 3 UP••• Tu••

14

r.....-_......16~30

100

'00

LQ"oos. APPROX

FlO. 4 Low•• Tu••

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so

100

240 -f1.-L:U--::~ APPROX

Fro. 5 RSCBIVING TUBE

15

IS : 10634 : 1986

Flo. 6 ASSEMBLY OFCHROMATOt.lRAPHIC TUBE

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IS I 10634 - 1986

c-4.PROCEDURE

0-4.1 SampliDI- Take a sample of the material weighing approxi­mately 10 g. Such a sample contains a total of about 250 I.U. vitamin A.

0-4.2 Saponification - Put the sample into the 200-n11 round bottomflask and weigh to the nearest 50 mg. Add 8 ml of potassium hydroxidesolution and 25 ml ethanol. Heat gently 011 a steam bath for one hour oruntil the saponification is complete, with a reflux condenser attached tothe flask. During this procedure, pass a slow current of oxygen-freenitrogen through the liquid.

C-4.3 EstractioD of Vitamin A - Add 50 ml water through thecondenser and cool the soap solution in rap water, Transfer the solutionto a separating funnel, using another 50 ml of water to rinse the flask.Extract the soap solution with successive portions of 100 and 50 ml diethylether by shaking. Wash the combined extracts in another separatingfunnel four times with 50 rnl of water ( the first time only by swirling, thefollowing three times by gentle shaking). Continue washing if the E-therla yer is still turbid.

C-4.4 EvaporatioD of the Solvent - Use the same flask in which thesaponification was carried out. Add the diethyl ether solution in twoportions. Heat on the water-bath ( 80 to 85°C). During the distillation,maintain a weak current of oxygen-free nitrogen until approximately5 ml is left. Then transfer the residue to a 50 ml conical flask, and rinsewith 15 to 20 rnl ether. Evaporate the ether with nitrogen, add SOIne

acetone and again evaporate the solvent.

0-4.4.1 Immediately take up the residue in 1-2 ml petroleum ether(if not clear, dry again with acetone) and introduce the solution on topof the upper chromatographic column with as little petroleum ether aspossible ( about 5 ml).

0-4.5 Chromatographic Separation of VitalDiD A Alcohol - Thechromatographic separation is carried out in two stages. For the firststage, only the upper column is used ( alumina). After the petroleumether extract ( from C-4.f.l ) has been brought on to the column, this ispassed through the adsorbent. Rinse the conical flask with 5 mlpetroleum ether and bring this amount on to the column. Rinse theflask with 5 ml portions of petroleum ether containing 4, 8 and 12 percentdiethyl ether ( vlu) respectively and use the washings for elution process.Discard all the elutes containing substances which are less stronglyabsorbed than vitamin A alcohol.

NOT J.; - Test for vitamin A with antimony trichloride in the elute contajnin.12 percent dicthyl ether. If the reaction is positive (in which cast' the aluminacontains roo much watf'r ), repeat the determination with a fresh column packing.

If)

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IS I 10634 - 1986

C-4.5.1 Then connect the second column (alkaline alumina) andelute with 5 1111 each of petroleurn ether containing 16,20 and 24 percentdiethyl ether (v'v), respectively. Finally, usc petroleum ether containing36 percent diethyl ether (VIi.!) until the vitamin A has been elutedcompletely. Collect the eluted fractions in the tubes graduated at 1 ml,Pirst, thoroughly mix the contents of each tube in order to obtain ahomogeneous solution. Do this by blowing SOIne air bubbles throughby means of the fine-tipped pipette. Then with the same pipette, removefrom each of the tubes approximately 0·3 n11 of the solution and withthese samples carry out the Carr-Price spot test ( using small test tube)with 0'5 ml antimony trichloride solution and 1 drop of acetic anhydride.

NorrB: - Ensure that during elution tho co lu rrms do not run dry but at tho samerime prevent, as much as posvible, the v.rrious petroleum ether fractions frommixing at the top of the first column. Onl~ v"ry little elute originating from thefirst column may be present on top of tht' second column.

0-4.5.1.1 Discard the fractions in which the Carr-Price spot test isnegative [generally those with 16 and ~o percent diethyl ether ( v/v )].

Nor ..:: - Special care should be taken in carry ing out Carr-Price spot test as thereaction i\ instantaneous ( takes 3 to 6 seconds only) and the blue colour developedis very unstable. It is, therefore, r ...-cornmended that addition of antimony trichloridereagvnt should be done quickly using blunt tipped pipette.

C-4.6 Spectrophotometric Determination of Vitamin A - Pipetteexactly 0·5 ml from each tube in which the Carr-Price spot test ispositive. Pool these in the 10-011 graduated flask, make up to the markwith petroleum ether used and mix. Make sure that the absorption at326 [Lm of the petroleum ether used does not change when 10 percentdiethyl ether is added. Use petroleum ether in the blank cell. Read theoptical density at the top of the extinction curve ( 324 to 326 fl.m ) using aI-em cell.

NOTE - It is recommended to occasionally compare the shape of the opticaldensity curve between 260 and 370 iJom with Mcrton-Stubbs ' ideal curve, This isdone to establish whether the separating capacity of the columns is sufficient. Thefreshly prepared adsorbents should always be tested in this way.

0-5. CA.LCULATION

Vitamin A (I.U.Jg) ~ 3~a

where

M = mals in g of sample, and

a -= optical density reading at the maximum,

17

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IS I 10634 - 1986

APPENDIX D

[Table I, Item (vii) (b), and Clause 7.1 ]

Q,UALITATIVE DETERMINATION OF VITAMIN A(ANTIMONY TRICHLORIDE METHOD)

D-O. PRINCIPLE

D-O.1 The sample is saponified with ethanolic potassium hydroxide andextracted with petroleum ether. The extract is reacted with antimonytrichloride and observed for appearance of a blue colouration whichindicates the presence of vitamin A.

D-l. REAGENTS

D-l.1 Absolute Ethanol - Ethanol may be purified as follows:

Reflux absolute ethanol for 30 minutes in presence of 10 g causticpotash and 10 g aluminium powder per litre of ethanol. The mixture isthen distilled in an all-glass apparatus with a fractionating columnof 50 to bO em length. Collect only middle fraction of the distillate,discarding the first and the last fraction each amounting to 5 percent ofthe total volume. The ethanol thus obtained should have the sameoptical absorption as glass distilled water in ultraviolet region.

D-l.2 Potassium Hydroxide Solution - 50 percent (mill).

D-l.3 Ether - peroxide free, redistilled (see IS: 336-1964*). Ethermay be maintained free from peroxides by adding wet zinc foilapproximately 80 ern" per litre, cut in strips long enough to reach at leasthalf way up the container, the zinc strips previously should have beencompletely immersed in dilute acidified copper sulphate solution for oneminute and subsequently washed with water.

D·l.~ Sodium Sulphate - anhydrous granular. "It shall not absorbvitamin A under conditions of use) and 10 percent solution shall not beacidic to methyl red indicator solution.

D-l.5 Chloroform - This may be purified as follows:

Wash the chloroform thrice with fresh 10 percent aqueous solutionof sodium thiosulphate in a separatory funnel. Dry the chloroform withanhydrous calcium chloride and filter. Distil the chloroform overanhydrous sodium thiosulphate in an all-glass apparatus with afractionating column of 70 cm length. Collect only middle fraction

·Specification for etber (,eLis,d).

18

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IS I 10634 - 1986

of the distillate, discarding the first 10 percent and last 10 percent of thedistillate.

Anhydrous sodium thiosulphate rnav he prepared from crystallinethiosulphate by careful heating between 105°C~ to 110°C and storing in adesiccator.

D-l.6 Aatimoay Trichloride SolatioD - Prepare by dissolving 113°4gantimony trichloride in 300 to ·lOO ml of chloroform. Add 5 g ofanhydrous calcium chloride and filter while hot. Dilute the filtrateto 500 ml with chloroform.

D..2. PROCEDURE

D-2.1 Weigh approximately 5 g of the material and transfer to anan-glass saponification flask, if necessary with a little alcohol. Add30 ml of ethanol (95 percent ,t v) and 5 1111 ef potassium hydroxidesolution with a jet tube for 3 minutes to replace the air. Then in a darkcorner, saponify the contents under I eJlux in an atmosphere of nitrogenover an electrically heated water bath for 30 to 40 minutes, Cool andthen add 30 ml of water. Transfer the contents quantitatively to dseparating funnel ( conical, squibb shaped, 250-ml capacity). W~sh theflask twice. with 10 1111 of water and add the washings to the separatingfunnel. Extract the saponified solution thrice. respectiv ply with 50, 20and 20 ml ether; combine the ether extract in another separating funneland wash this with 50 ml of ice cold water containing a little sodium acidsulphate ( NaHSO,,) or potassium acid phosphate ( KH~PO, ) Just enoughto neutralize the alkalinity of the extract. Repeat the washing with onlyice cold water till the washings are neutral to phenolphthalein.

Transfer the ethereal extract to a stoppered measuring cylinder( 100 ml ), rinse the separating funnel with a little ether and then addthis to the cylinder. Add more ether to make the volume to 100 mlmark. Then add anhydrous sodium sulphate ( 15 grams), mildly shakea little and allow it to settle in a dark cool place. Evaporate the etherunder moderate heat and reduced pressure to obtain a residue. Dissolvethe residue in a small amount of chloroform. Take 2 ml of thechloroform solution, add a drop of acetic anhydride and then addrapidly 0·5 rot of antimony trichloride solution.

D-2.2 The material shall be considered to have passed the test if a blueeolouratien appears immediately indicating the presence of vitamin A.

NOTB - Special care should be taken in carrying out this test since the reactionis spontaneous ( takes 3 to 6 second. only) and the blue colour developed is veryunstable,

19

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IS I 10634 • 1986

APPENDIX E

( Clause 7.1 )

TEST FOR SOLID FAT INDEX.

E-O. GENERAL

E-O.l Solid fat index (dilation value) is an empirical measure of thesolid fat content. It is calculated from the specific volumes at varioustemperatures utilizing a dilatometric scale 'graduated in units of ml x1 000. Results are. therefore. expressed as melting dilation in ml.kg offat.

£-0.2 The method is applicable to margarine oils, shortenings andother fats with a solid index of 50 or less at IO'JC. The method isempirical and departures from the procedures may cause variations inresults,

~~1.. APPARATUS

E-l.1 ResistaDt Borosilicate Glass Dilatometers - Constructed inaccordance with the specifications given in Fig, 7. The stem should bemade from precision bore capillary tubing graduated in O·OO5-mlincrements from 0 to 1·400 ml, with an overall Rcc-uraey of at least± 0·00, ml, The scale shall he marked 0 to 1-400 in intervals of 50.The dilatorneters shall have identification numbers on the stems andstoppers.

E-l.2 SpriDls - To fasten dilatorneter stoppers.

E-l.3 Clamps - For holding the dilatometers in the constant tempera­ture baths,

E-l.t CODstaat Temperatare Water Baths - accurate to ± o·osCieequipped to provide adequate circulation.

E-I.5 Vacaam Pump - capable of reducing pressure to 2 mmHg orless.

E-l.' Stopcock - 2 mm ID capillary 2-way stopcocks with a burettetip made of borosilicate glass,

E-l.7 Cemeat

20

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IS : 10634 • 1986

--....-~~8 00

25APPROX

,SAPPRQX 100

APPROX

All dimensions in millimE-tres.

Flo. 7 DILATOMBTEIt

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IS I 10634 • 1986

E·2. REAGENTS

E-2.1 Pota••iuDl Dichromate Indicator Solation - one percent inwater.

E-2.2 High Vacuum Grease - - silicone type.

E-2.3 Petroleum SolveDt

E-2.4 Mercury -- distilled.

E·3. CALIBRATION

E-3.1 All new dilatometcrs shall be checked for accuracy as follows:

a} Thoroughly clean and dry the dilatometer;

b) Clamp the dilatorneter securely in an inverted position;

c) Clamp the capillary stopcock in place at the end of thedilatometer stem and make a seal with cement;

d) After the cement has hardened, immerse the tip of the stopcockinto a reservoir of clean mercury which is at room temperature;

E') Using vacuum, draw the mercury into the dilatometer stem untilthe calibrated portion is fun;

f) Successively withdraw 0·200 rot portions of mercury into atared 50-nll beaker and record the mass; and

g) Calculate the true volume in rnl contained in each measuredscale intervals as follows:

mass of mercuryX sp vol of mercury at Tn X I 000

(final- initial) scale reading

where

TR = room temperature.

1 rnl - 1 000 in scale reading.

NOTE - In order to meet the specifications or thil method, the dilatometerseale should be accurate to 0·005 ml or If·•• ( I scale graduatioD ) from 0 to I 400. Itis necel,ary to draw eorrecrlon curvea from the calibration data for tholedilatometere which do not meet Ipecification. and corrected readinl mUlt be used tocalculate the .oUd rat index.

22

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IS I 10634 • 1186

E-4. PROCEDURE

£-4.1 FilliDg the Dilatometer

E-4.1.1 Deaerate about 50 ml of the indicator solution for 3 minutesin a 250 ml filter flask or a strong oil sample bottle at a pressureslightly above the vapour pressure of the solution at the temperatureof deaeration. ( The vapour pressure of water at 25°C is 24 mrn ). Theindicator may also be deaerated by vigorously boiling for 15 minutes atatmospheric pressure but should be cooled to room temperature beforeuse.

E-4.1.2 Heat the bakery shortening sample to 80° C and deaerate in a250 ml filter flask or strong sample bottle at a pressure of 2 mmHg untilno more gas bubbles are seen, for at least 2 minutes, The sample mustbe maintained in a liquid state and agitated vigorously during deaeration,

NOT}f~ - The indicator and sample should be used as soon as possible after theyhave br-en dear-ran-d, The fat should bp comp lete lv melted. Even stightcryst.l1h7ation occludes air,

E-4.. 1.3 Pipette 2 ml of the indicator solution into the dilatometer bulb.Lubricate the stopper lightly with silicone grease and weigh the assembleddilatometer to the nearest 0'01 g on a torsion balance.

E-4.1.4 Carefully overlay the indicator with the melted sample and filluntil the sample overflows. Insert the stopper so that the indicatorsolution rises to approximately the 1 200-rnark of the stern when thestopper is securely sealed. ("rhe reading should be I 200 ± 100 at 60 JC;

if not, the deterrnination should he repeated ).

E-4.1.5 Wash the fat from the outer surface of the dilatometer withpetroleum sol vent. Attach the retaining springs and reweigh thedilatorneter when the solvent has evaporated.

E-4.2 Measurement of Thermal ExpaDsioD

E-4.2.1 Immerse the dilatometer to the 300-rnark in the 60°C bath andrecord reading after 15 minutes and then at 5 minute intervals until thechange is less than 2 units in 5 minutes. ( Rechecks of rhe 60 J C readingat the end of the determination should agree with the 60vC referencereading). Significant variations indicate faulty technique.

E-4.2.2 Transfer the dilatometer to the 37·SoC bath and immerse tothe 300-mark. Read level of indicator at intervals of 5 minutes until thechange is less than 2 units in 5 minutes. Record the readings.

NOTE -It is necessarv for the sample to be completely melted at the lowertemperature. If any lIf"eding or clouding of the sample occurs, rvrnelt the samplein a 60°C bath and raise the temperature of the other bath. If the reference bathtemperatures are changed, appropriat£· subsritution must bt, made in the calculation•.

23

Page 33: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

IS I 10634 - 1986

£-4.3 CODdltioDiag of the Sample

E-t.3.1 Transfer the dilatometer to the O·C bath and immerse to the300-mark and hold for 15 minutes.

E-f.3.2 Transfer to a 15·0:> C bath and hold for 30 minutes.

E-t.3.3 Transfer back to O~C bath and hold for 15 minutes.

NOTE-If In ice bath is used, provisions should be made (or adequate watercirculation.

E-4.4 Measaremeat of DilatjoD

E-4.4.1 Transfer the dilatemeter from the O"'C bath to a bath at thelowest desired temperature. Immerse to the gOO-mark and recordreading at 30 minutes.

E-4.4.2 Repeat at the next highest temperature and so on untilreadings have been obtained at all of the desired temperatures.

E-4.5 CalculatioD

Solid fat index ( at 15°C ) = ( Tata 1dilation) -[ Thermal expansion X (60 - 15 ) ]

Thermal expansion of sampleper degree C in rol/kg

Total dilation between lS'"C R R VCand 110°C in ml/kg = _~-=--15 - 15

M

where

VCI 3 :::a volume correction for expansion of glass. and waterat 15JC;

R t5 -= dilatometer reading at 15'- C;

RIO = dilatometer reading at 60°C; and

M = mass in g of the sample.

NOTE I - VC from the Table 2 represents the combined correctiODir"r the expansion of glass and water and applies to borosilicate ,Ia••only. If dilatorneter is made of Ilass other than boro,llicate, thecorrections should be redetermined,

NOT. 2 - The liquid thermal expansion is basic Cor calculatiD, thesolid rat indt'x. I t should, therefore, bs accurate.

24

Page 34: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

IS : 10634 • 1986

Repeat analyses have shown values of 0'83 to 0-85 mljkg to benormal for cottonseed oil, soyabean oil, lard and tallow. Lauric acidells, such as coconut, have values of 0'S5 to 0-S7 ml/kg. If determinedvalues are abnormal, the analyses should be repeated, Standard thermalexpansions may be applied in routine determinations where results areused within an organization, provided they are checked periodically byactual measurement.

TABLE 2 VOLUME CORRECTIONS

BA'l'B 60Ge REA nrxoTB)lPBRATORB ,,--_____-------.-.-J...------ __.______~

°C 1000 1100 1200 1300 1400

0 22'0 20'3 ISb 169 15 25 22'2 205 18'7 li oO 15'3

10 21'8 20 1 184 16 7 15'115 21°0 19'5 Ii 8 1(l'2 14620 19'8 18°4 168 15°3 13-825 18'4 17-0 156 14'1 12 730 16°6 15°3 14'0 12°7 11°435 14°4 13'3 12 2 11'1 100

40 12'0 11°0 102 goZ 8°345 g... 8°7 8°0 - ? 6°5, -50 66 601 5'6 5 1 4-555 3°2 3'0 2'8 2°5 2-360 0 0 0 0 0

25

Page 35: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

IS I 10634 • 1986

(Con'i,.,dIr.. pal' 2 )

M",.6", R,pru,nlin,ASSISTANT DIRECTOR (AQRI ENOO) Indian Council of Agricultural Research Institute,

New DelhiAS81STANT DIRECTOR GENERAL Central Committee for Food Standard. (CCFS)

(PFA) (Ministry of Health and Family Welfare),New Delhi

ASSI8TANT SECRETARY ( PFA) (.AII,rnat, )SUBI V. K. BANSAL Central Organization for Oil Industry and Trade,

BombaySHRI H. P. GUPTA (Alt,rn/d,)

SHRI P. V. GUJAItATHI Khadi and Village Industries CommissioD,Bombay

SBRI G. K. SOOD

SDRI M. S. THAKUR

SnBI R. D. SHB:NOIL

DR I. S. SHEMOI.IKARDR RAMF:~lI BHATr ( Altertuu« )

DR I. A. SU)()IQUI Directorate of Vanaspari, Vegetable Oils andFatl (Ministry of Food &. Civil Supplies),New Delhi

Vanaspad Manufacturers' AssociatioD of India,New Delhi

Indian Soap and Toiletries Makers' Association,Bombay; 4nd Godrej Soapi Ltd, Bombay

SSRI S. D. TBIR UMALA RAO Oil Technological Research Institute, AnantapurSHRI D. ATCJiYUTA RAMAYYA ( AII,rna',)

SBRI M. D. WASNIK Directorate of Oilseed. Development, HyderabadDR RAJVIR SIKGH (AII,r,..',)

SURI V. K. B. NAla (Alternate)SHIU R. D. KAwA'rRA Directorate General of Technical Development,

New DelhiDB V. V. S. MANI Hindustan Lever Ltd, Bombay

SURI K. S. JAN ARDIf AS AN (Allernat,)SRRI R. K. MArtPHATIA Indian Paint Association, Calcutta

SHIH RADI~ SARK,\U, (Alternat,)DR N. L. MUI\TY rrata Oil Mill. Co Ltd, Bombay

Oil A. D. SHl'fOL~ ( Altemat« )DR S. M. PATEL Oil Technologists' Association of India, Kanpur

PRor V. V. R. SUBRAIfMANYAM ( Alt",.41, )DRJ. V. PRABJIAKAR. Central Food Technological Research Institute

(CSIR), My.oreIndian Confectionery Manufacturers' Association,

New DelhiIndian Council of Medical Research, New Delhi

26

Page 36: IS 10634 (1986): Bakery Shortening - Public.Resource.Org · Amend No.1 to IS 10634: 1986 F·1.1.3.1 Methodusingpersulphate for oxidation F·1.2.3.1.1 Calibration - Transfer 1, 2,

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