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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. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 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 14125 (1994): DL-Tartaric Acid, Food Grade [FAD 8: Food Additives] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 1412&: 1984 ~lfACP ~-GTtn:cp ~, ~Rf V6 - ~ Indian Standard DL-TARTARIC ACID, FOOD GRADE SPECIFICATION C 815 1994 BUREAU OF INDIAN STANDARDS MANAK BHAVAN. 9 BAHADUR SHAH lAFAR MARG NEW DELHI 110002 June 1994 Price Group 2 ; AMENDMENT NO.1 APRIL 2006 TO IS 14125: 1994 DL-TARTARIC ACID, FOOD GRADE - SPECIFICATION (Page1,clause2)- Substitute'1699:1995 for'1699: 1994'. t ( Page 1,clauseS, line S ) - Substitute 'IS 1699 : 1995' for 'IS 1699 : 1994'. [Page2, Table 1,SINo.(vii),col4]- Substitute'ISofIS1699:199" for'15 ofIS1699:1994'. (Page2, Table 1)-Insertthefollowingatthe endofthe table: sa~o. Chu8derlltle Require... MetbcMIofT...fao (I) (2) (3) (4) 6.yJii) Lead(uPb),mg!k& 2 ISof181699:1995' Mea (PAD8) ReproaraPbyUnit,81S.NewDelhi,India Food Additives SectionalCommittee. FAD 8 FOREWORD This Indian Standard was adopted by the Bureau ofIndian Standards after the draft finalized by the Food Additives Sectional Committee had been approved by the Food and Agriculture Division Council. With the increased production of processed foods, manufacturers have started adding a larae number ofsubstances. generally in small quantities, to improve the appearance, flavour, texture or storage properties of the processed foods. As certain impurities in these substancescould be harmful, it is necessary to have a strict quality control of these food additives. A seriesof standards has, therefore, been prepared by this Bureau to cover purity and identification of these substances. These standards help to check purity at the stage ofmanufacture, for it is extremely difficult ( and in many cases impossible) to detect the impurity once these substances have been added to the processed foods. Besides, these standards are intended to guide the indigenous manufacturers in making their product conform to specifications that are accepted by scientists, health authorities and international bodies. DL-Tartaric acid is alia known as 2, 3-dihydroxysuccinic acid. Its chemical formula, structural formula and molecular mass are given below: Chemical Formula Structural Formula Molecular Mass HOOC--CHOH--CHOH--COOH 150·09 In the preparation ofthis standard considerable assistance has been derived from the FAO/WHO, Food and Nutrition Paper No. 4- 'Specification for identity and purity ofthickening agents, anticaking agents, antimicrobials antioxidants and emulsifiers' published by FAO, Rome 1984. For the purpose ofdeciding whether a particular requirement ofthis standard is complied with, the final value, observed orcalculated, expressing the result ofa test or analysis, shall be rounded off in accordance with IS 2 : 1960'Rules for rounding off numerical values ( revised )'. The number of significant places retained in the rounded off value should be the same al that ofthe specified value in this standard. IS 1.-125:1"4 Indian Standard DL-TARTARIC ACID, FOOD GRADE SPECIFICATION 1 SCOPE 4.3 Marklnl This standard prescribes the requirements and the methods ofsampling and test for d/-tartaric acid. 4.3.1 Each containershallbe ICllibly and indelibly food grade. marked to give the following information: 2 REFERENCES a) Name ofthe material including the words The following Indian Standards are necessary 'food grade'; adjuncts to this standard: b) Source ofmaunfacture; IS No. Title c) Minimum net mass ofthe contents; 1010: 1992 Water for general laboratory use d) Batch or code number; ( thirdrevision) 1699: 1994 Methods of sampling and test e) Date ofmanufacture; and for food colours (first rev/sinn) f) Any other details required as per the Standards of Weights and Measures 3 REQUIREMENTS i Packrged Commodities) Rules, 1977/ 3.1 Description Prevention of Food Adulteration Rules, 1955. Db-Tartaric acid shall be either in the form of colourless or transluscent crystals or a white :1: crystalline powder. It shall be odourless and have 4.3.2 BISCertlficatton Marking an acidic taste. Each container may also be marked with the Standard Mark. 3.2 Idfntffieation 3.2.1 Solubi/ity 4.3.2.1 The use ofthe Standard Mark isgoverned by the provisions ofBureau of Indian Standards It shall be freely soluble in water and sparingly Act, 1986and the Rules and Regulations made soluble in ethanol. thereunder. The detailsofconditionsunderwhich a licence for the use of the Standard Mark may 3.1.2 A ten percent solution has no optical be given to manufacturers or producers may be activity. obtained from the Bureau ofIndian Standards. 3.2.3 Its solutions give a positive test for tartarate as given below: 5 SAMPLING tA fewmilligrams of tataric acid in solution when added to a mixture of 1Sml of pyridine Representative samples of the material shall be and S ml acetic anhydride, result in drawn and conformity of the material to tho production ofan emerald green colour.' requirements of this specification shall be determined according to the procedure prescribed 3.3 The material shal! conform to the require- in 4 ofIS 1699: 1994. ments given In Table 1. 6 TEST 4 PACKING, STORAGE AND MARKING 6.1 Tests sbalJ be carried out by the methods as 4.1 Packiog specified in 3.2 and col 4 ofTable 1. The material shall be securely packed in well filled containers with as little airspace as possible. 6.2 Quality of Realeats The container shall be such as to preclude contamination of the contents with metal or Unless specified otherwise, pure chemicals and other impurities. distilled water (.re~ IS 1070: 1992) sball be employed in tests, 4.1 Storale NOTE- 'Purechemicals'shall mean chemicals tbat The material shall be stored in a cool and dry do not contain impurities which affect th e place so as to avoid excessiveexposureto beat. experimentalresultl. 1 IS 14125: 19'4 Table 1 ReflDlre....tI01DL-Tartarlc Acid, Food Grade ( Clause, 3.3 and 6.1 ) 81No. Charederlltlc RequirelDeat Metbod01Tilt,ReIto ( 1) ( 2) ( 3) (4) i) PurityalC.H.O.(ODdry basis ), percent by 99'5 A-I mass,Min 11) LOIsondryinl, percent by mass,ondryioa 0-5 at lO'·Cfor3houriover P,O••MQJC iii) Sulphatedash, percent bymass,Mu &1 A-2 iv) Readilyoxidizablesubstances A-3 .·0 a) Fumaricacid, percent by maSI, Ma~ b) Maleicacid, percentby mass, Ma1( 0·05 v) Sulphate,percent by mass, Max O'OS A-4 vi) Heavymetals (as Pb), ml/ka, Max 10 A-S or vii) Anenic(as As),maika, Max 3 15 IS 1699:1994 ANNEX A [ Table 1, Sl No. (i), (iii), (iv), (v) and (vi) ] METHOD OF TEST FOR DL-TARTARIC ACID, FOOD GRADE A-I DETERMINATION OF PURITY A-2.3 Calculation A-I.l Rea.ent Sulphate ash, percent bymass = Z~ x 100 A-I.I.t Sodium Hydroxide - 1N. where A-I.l.% Phenolphthalein M: == mass, in g, ofthe residue; and Dissolve 0·2 g of phenolphthalein in 60 ml of MI == mass, in g, ofthe material taken for 90 percent ethanol and add sufficient quality of the test. water to produce 100 ml ofthe solution, A-I.2 Proeedure A-J DETERMINATION OF FUMARIC AND MALEIC ACIDS Weigh accurately about 2·0 g of tartaric acid, previously dried over phosphorus pentoxide for 3 h. Dissolve it in 40 ml of water, and titrate A-3.t Reagents with the sodium hydroxide using phenolphthalein as indicator. Each ml of I N sodium hydroxide A-3.I.t BufferSolution A is equivalent to 75-04 mg of C,H 60,. Dissolve 74'S8 ofpotassium chloride in SOO ml A-l DETERMINAnON OF SULPHATED of water in a I OOO-mi volumetric flask, add ASH 100 ml ofhydrochloric acid, and dilute to volume with water. A-2.1 Reagent A-3.1.2 Buffer Solution B A-l.I.! ConcentratedSulphuric Acid Dissolve 171-0 8 ofdibasic potassium phosphate A-1.1 Procedure K.HPO•• 3HsO, in I 000 ml of water and add Weigh accurately about 2g ofthe material in a monobasic potassium phosphate, KH.PO. until tared crucible, Ignite, genlly at first, until the thepH is exactly 7'0. material is thoroughly charred, cool and moisten the residue with I ml ofsulphuric acid and ignite 1\-3.1.3 Maximum Supprellor Bently till 'the carbon is completely combusted, Cool the crucible in a desiccator and weigh, Dissolve with the aid of8 magnetic stlrrer, I I ofgelatin in 65 ml ofhot, boiled water and after NOTE- Carryoutthe ilnition In 8 place pro tected cooling add 3S ml of anhydrous etbaaoJ as form air currents and use as low a temperature.1 ~ssibie toeffectthecombustionofcarbon. preservative. 2 IS 14125: 1994 A-3.1.4 StandardSolution where C .. concentration, in mp per ml, ofcombined Weilb accurately about 20g of the sample, maleic acid and fumaric acid in the 100mg of fumaric acid of the highest purity standard solution. available and 10mgofmaleic acid of the highest purity available and transfer ~into a SOO ml Mass of maleic acid = SOOC' xiu'/(i8'- iu' ) volumetricflask. Add 300 ml ofsodiumhydroxide where solution (4·3 g ofsodium hydroxide dissolved in C'= concentration, in mg per ml, ofmaleic water to make 100 n11) and a few drops of acid in the standard solution. phenolphthalein solution and then continue the neutralization with sodium hydroxide solution to Mass offumaric acid a faint pink colour that persists for at least 30 in the sample = MR!'\S of combined seconds. Dilute to volume with water and mix. maleicacid and fuma ric acid - Mass of maleic acid A-3.1.5 Sample Solution A-4 DETERMINATION OF SULPHATE Transfer about 4 g of the sample accurately weighed into a 100 ml volumetric flask. and A-4.1 Reagentl dissolve in 25 ml ofwater. Add phenolphthalein solution and neutralize with sodium hydroxide A-4.1.1 Sulphuric Acid- 0·01 N. solution as directed for the standard solution. Dilute to volume with water and mix. A-4.1.1 Hydrochloric Acid- 3 N. A-3.2 Procedure A-4.1.3 BariumChloride - 10 percent solution. Transfer 2S·0-ml portion ofsample solution into A-4.2 Apparatus separate lOO-ml volumetric flasks. Dilute one A-4.2.1 Nessler', Cylinder, - SO-ml capacity. flask (sample ~) to volume with buffer solution B and dilute to volume with water. A-4.2.2 Standard Measuring Flask - 100 ml capacity. Rinse a polarograph cell with portion of sample A-4.2.3 Pipettes- I-ml capacity A, add a suitable volume ofthe solution to the cell. immerse it in a water bath regulated at 24·5° A-4.3 Procedure to 25·5°.add 2drops of the maxima suppressor, and then deaerate by bubbling nitrogen through Weigh accurately about 0-4g ofthe sample and the solution for at least 5 minutes. Insert the dissolve in 30-40ml of water in a Nessler's dropping mercury electrode (negative polarity) cylinder. Add 1ml of 3 N hydrochloric acid, of a suitable polarograph, adjust the current 3 ml of barium chloride solution and sufficient sensitivity asnecessary and record the polarogram water to make SO ml. Mix, allow to stand for from -0·1 to -0·8 Vat the rate of0·2 V per 10 minutes and compare the turbidity. if any, minute using a saturated calomel electrode as with that produced in a solution containing the reference electrode. Transfer 25'0 ml of the 0·5 ml of0·01 N sulphuric acid in the control. standard solution into a IOO-ml volumetric flask and dilute to volume with buffer solution A. A-5 DETERMINATION OF HEAVY METALS Obtain the polarogram ofthis standard (standard A) in the lame manner as directed for sample .4. A-S.t RealeDts In each polarogram determine the height of the maleic acid plus fumaric acid wave occuring at A-5.1.1 AmmoniaSolution the half-wave potential near -0·56 V, recording Dilute 400 ml of ammonium hydroxide (28 that for the sample as iu' and thatfor the standard percent) to 1000 ml with water. as il'. A-S.t.l Hydrochloric Acid - 10percent. In the same manner obtain polarograms from sample B and standard B, except record the A-S.t.3 LeadNitrate Stock Solution polarogram from -1·05 to 1·7V at the rate of o1Vper minute. In each polarogram determine Dissolve 1581S mg of lead nitrate in 100 ml of the height of the maleic acid wave occuring at water containing 1ml ofnitric acid. Dilute with the half-wave potential near -I·33 V. recording water to I000 ml and mix. Prepare and store the that for the sample 8S iu' and that for the solution in lead-free 81asscontainers. standard as il'. A-S.l.4 StandardLead Solution A-3.3 CalculatloD Dilute 10 ml of lead nitrate stock solution, accurately measured, with water to 100 ml. Each Mal. ofcombined maleic ml of the solu1t'i.on so prepared contains the acid and fumaric acid == SOOexiu/(i......iu) equivalent of 10 oflead ion (Pb). 3 IS 14125: 1994 A-S.I.S Nitric Acid- 10 percent. ignition. After the substance i. thoroughly carbonized, add 2 ml of nitricacid and 5 drops A-S.t.6 Sulphuric Acid- 94·' to 95·5 percent. ofsulphuric acid, and cautiously heat until white fumes are evolved. Then ignite, preferably in a A-5.1.7 Acetic Acid - 6 percent. muffle furnace, at SOO to 600°C until the carbon is completely burnt off. Cool and add 4 ml of A-S.I.8 Hydrogen Sulphide dilute hydrochloric acid. Cover the crucible and digest sample on a steam-bath for 10 to IS A saturated solution of hydrogen sulphide made minutes. Uncover, and slowly evaporate tho by passing HIS in cold water. sample to dryness on a steam-bath. Moisten the residue with one drop ofhydrochloric acid, add A-5.2 Procedure 10ml ofhot water and digest for 2 minutes. Add dropwise, ammonia solution until the solution is A-S.2.1 Solution A just alkaline to litmus paper. Dilute with water to 25 ml and adjust the pI'! to between 3·0 and Take 2 ml ofthe standard lead solution in SO ml 4·0 (pH indicator paper) by the addition of Nessler tube and add 23ml ofwater. Adjust the dilute acetic acid. Filter if necessary and wash pH to between 3·0 to 4·0 byaddition ofacetic the crucible and the filter paper with 10ml of acid or ammonia solution. Dilute with water to water. Transfer to a 50 ml Nessler tube. Dilute 40 ml and mix. the combined filtrate and washings with water to 40 ml and mix. A-~.2.Z Solution B Take 2g ofthe sample. accurately weighed, in a A-5.2.3 To each tube add 10 ml of freshly suitable crucible. Add sufficient nitric acid to prepared hydrogen sulphide. Mix and allow to wet the sample, and carefully ignite at a low stand for Sminutesand view over a white surface. temperature until thoroughly charred, covering The colour ofSolution B shall not be darker than the crucible loosely with a suitable lid during the that ofSolution A. 4