(1988): Methods of Sampling and Test for Oils and Fats, Part II
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इंटरनेट मानक 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. “जान का अधकार, जी का अधकार” “परा को छोड न 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 548-2-9 (1988): Methods of sampling and test for oils and fats, Part II: Purity tests, Section 9: Test for presence of Karanja (Pungam) oils in other oils [FAD 13: Oils and Oilseeds] “ान $ एक न भारत का नमण” Satyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” “ान एक ऐसा खजाना > जो कभी चराया नह जा सकताह ै”ै Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” (Reaffirmed 2010) IS : 548 ( Part 2lSec 9 ) - 1988 ( Reaffirmed 1994 ) Indian Standard METHODSOFSAMPLINGANDTEST FOROILSANDFATS PART 2 PURITY TESTS Section 9 Test for Presence of Karanja ( /+ngam ) Oil in Other Oils ( Fourth Revision ) Second Reprint APRIL 1998 UDC 665.21.3~543t665.325.37 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC NEW DELHl 110002 Gr 2 April I989 IS:548(Part2/sec9)-1988 Indian Standard METHODS OF SAMPLING AND TEST FOR OILS AND FATS PART2 PURITY TESTS Section 9 Test for Presence of ( Karanja Pungam ) Oil in Other Oils ( Fourth Revision ) 0, FOREWORD 0.1 This Indian Standard ( Part 2/Set 9 ) ( Fourth Section 13 Test for the presence of groundnut Revision) was adopted by the Bureau of Indian oil [ Bellier turbidity temperature Standards on 30 May 1988, after the draft finalized test ( Acetic acid method ) 1 by the Oils and Oil Seeds Sectional Committee Section 14 Test for the presence of Kusum oil had been approved by the Chemical Division and other oils containing cyanoge- Council and Agricultural and Food Products nit compounds Division Council. Section 15 Test for the presence of castor oil 0.2 This standard was first published in 1954 and Section 16 subsequently revised in 1964 as Part 1 and it Test for the presence of Neem oil covered methods of sampling, physical, chemical Section 17 Test for the presence of other oils and qualitative tests. in castor oil 0.21 In view of periodical review of qualitative Section 18 Test for the presence of animal fat tests for detection of adulteration in oils and fats, vegetable oils ( phytosterol it was decided to cover such tests in Part 2 of Eetate melting point test) this standard and IS : 548 ( Part 2 )- 1976* was Section 19 Test for the presence of oil soluble accordingly published. colours in oils and fats 0.2.2 It was felt that additional purity tests 0.3 Section 9 of IS : 548 ( Part 2 )- 1976* has now and the existing test methods when revised should been brought out as a separate standard after its be covered in the form of separate test methods revision. In the revised standard, two methods and not added as amendments to the standard of tests have been prescribed for detection of ( that is, Part 2 ) since it would create confusion. Karanja oil in other oils. The earlier prescribed The tests covered under various sections of method was not very sensitive and, therefore, an IS : 548 ( Part 2 )-1976* are as follows: additional TLC method which is more sensitive, Section 6 Test for the nresence of sesame oil has been specified in the revised standard. Subse- ( modified Biudouin test ) quently, Section 9 of IS : 548 ( Part 2 )-1976* is being deleted through an amendment. Section 7 Test for the presence of cottonseed oil ( Halphen test ) 0.4 Karanja or Pungam ( Pongamia Glabra, Section 8 Test for the presence of linseed oil Pongamia Pinnata )-Oil is a commercial non- ( Hexabromide test ) edible oil. It is usually cheaper than many other vegetable oils and can perhaps be used for adult- Section 9 Karanja Test for the presence of erating other dark-coloured and odoriferous oils ( Pungam ) oil and other oils con- in raw form and light coloured oils after taining phenolic substances refining. Section 10 Test for the presence of argemone oil by paper chromatographic 0.5 In reporting the result of a test or analysis method made in accordance with this standard, if the final value, observed or calculated, is to be Section 11 Test for the presence of hydrocya- rounded off, it shall be done in accordance with nit acid IS : 2-1960t. Section 12 Test for the presence of mineral oil *Methods of sampling and test for oils and fats: *Method of sampling and test for oils and fats: Part 2 Purity tests. Part 2 Purity tests. j-Rules for rounding off numerical values ( revised 1. 1 IS :.54S ( Part 2/Set 9 ) - 1988 1. SCOPE 4.2.2.1 Chloroform 4.2.2.2 Methanol 1.1 This standard ( Part 2/Set 9 ) prescribes the methods of test for detection of Karanja 4.2.2.3 n-Hexane ( Pungam ) oil in other oils. 4.2.2.4 Diethyl ether 4.2.2.5 Acetic acid 2. GENERAL 4.2.2.6 Formic acid 2.0 Two methods have been prescribed, namely, antimony trichloride and thin layer chromato- 4.2.3 Oil Samples graphy ( TLC ) method. In case of any dispute, 4.2.3.1 Raw Karanja oil the TLC method shall b:: the referee method. 4.2.3.2 Alkali-refined and bleached Karanja oil - Raw Karanja oil is relined with 15 percent 3. lW;;Wg; ‘, ( ANTIMONY TRICHLORIDE aqueous sodium hydroxide solution ( 5 percent excess over the theoretical requirement ) by stirr- 3.0 General - The non-saponifiable component ing mechanically for 30 min at room temperature, of this oil reacts with antimony trichloride to and filtered. Refined oil is bleached with 3 per- form yellow to orange coloured complexes. cent bleaching earth and 1 percent active carbon at 120°C for 15 minutes with stirring and filtered. 3.1 Reagent 4.2.3.3 Acid-refined and bleached Karanja 3.1.1 Antimony Trichloride Solution - 20 per- oil - Raw Karanja oil is stirred mechanically for cent ( m/v ) in chloroform. The reagent is pre- 30 minutes at 40°C with 1 percent concentrated pared by weighing antimony trichloride crystals, sulphuric acid and filtered. The refined oil is adding to chloroform and shaking for a few bleached as in 4.2.3.2. minutes till the crystals dissolve. 4.2.3.4 Alcoholic alkali-refined and bleached Karanja oil - Raw Karanja oil is refined with 0’3 3.2 Procedure - Take one drop of the oil percent ethanolic ( 95 percent ) sodium hydroxide sample in a small test tube or in a depression solution ( oil : alcoholic alkali, 1 : 1 ) for 45 of porcelain tile. Add 1 to 2 ml of antimony minutes at room temperature with mechanical trichloride reagent. An immediate characteristic stirring. The oil layer is separated. The above canary yellow to orange yellow colour shows the process is repeated with 0’1, 0’ 1 and 0’3 percent presence of Karanja ( Pungam ) oil in the sample. alcoholic sodium hydroxide in three stages. After 3.3 Sensitivity - This test is sensitive to the filtration, the refined oil is bleached as in 4.2.3.2. extent of 3 percent of Karanja (Pungam ) oil in 4.2.3.5 Alcohol-refined Karanja oil - Raw other oils. Karanja oil is stirred mechanically for 45 minutes with 95 percent ethanol ( oil : alcohol, 1 : 3 ) at 4. METHOD II ( THIN LAYER room temperature. The oil layer is separated CHROMATOGRAPHY METHOD ) and the process repeated once again. The refined oil is bleached as in 4.2.3.2. 4.8 It is a sensitive and specific method for detec- tion of adulterationor contamination with Karanja 4.2.3.6 Other oils used for preparing artificial oil, either raw or refined with alkali, acid, ale+ mixtures are genuine raw oils. ho1 or alcoholic alkali and bleached. The method is based on the separation of minor constituents 4.3 TLC on Micro Slide present in Karanja oil by thin layer chromato- graphy ( TLC ) and their visualization in ultra- 4.3.1 Apparatus violet light. 4.3.1.1 Micrb slides 4.1 outline of the Method - A solution of 4.3.1.2 Coupling iaior a suitable chamber - the oil sample to be tested and of the pure refe- for developing micro slides. rence oil are applied on micro slide or regular glass plate coated with silica gel and developed 4.3.1.3 Graduated micro pipettes or syringes - with a solvent mixture. In ultraviolet light, an 10 ~1 and 100 ~1 capacity. additional flourescent spot, having a Rt value 4.3.1.4 Ultraviolet lamp ( 366 nm maximum of about 0’27, is seen when Karanja oil is present. emission ). 4.2 Material 4.3.1.5 Stoppered conicalflask - 250-ml. 4.2.1 Adsorbent - Silica gel containing a 4.3.1.6 Glass tube - ( 9 x 4 cm ) or a suitable binder ( silica gel ‘G’ for use in TLC ). size beaker. 4.2.2 Solvents - Laboratory reagent grade.