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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 15623 (2005): Melamine (2 , 4, 6 triamino 1, 3, 5 triazine) [PCD 12: Plastics] “!ा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 15623:2005 WwfbmmF *(VL6’E@%+rl,3,5m)- n IIY Indian Standard MELAMINE (2, 4, 6 TRIAMINO 1, 3, 5 TRIAZINE ) — SPECIFICATION ICS 71.080.90 0 BIS2005 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 octoher 2005 Price Group 3 Plastics Sectional Committee, PCD 12 FOREWORD This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Plastics Sectional Committee had been approved bythe Petroleum, Coal and Related Products Division Council. Melamine (2, 4,6 Triamino 1,3, 5Triazine )isabasechemical, available infine powder form and usedto prepare melamine formaldehyde resin of different M: F ratio depending upon the application of resin. The melamine formaldehyde resin so produced is further modified that is either methoxylated or butylated to get different variety of resin to suit its application. The melamine formaldehyde resin m derivative so produced finds application as reactive component during the manufacture ofpaint, adhesive, lacquer, textile treatment chemical, and super-plasticizer asconstruction chemicals incement industries. Conversion of melamine formaldehyde resin into moulding powder, and use of melamine formaldehyde resin in decorative laminate, plywood sheet, medium density particle board, high density particle board and veneer board iswell known. Recent development shows that melamine and its derivatives like melamine polyphosphate, melamine-cyanurate with additives find applications as flame retardant for plastics and polymers and also as fire extinguishing dry chemical powder due to its high heat capacity and decomposition at very high temperature. For the purpose of deciding whether a particular requirement of this standard is complied with the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS2: 1960 ‘Rules for rounding off numerical values (revised )’. The number ofsignificant-places retained inthe rounded off value should be the same as that of the specified value in this standard. IS 15623:2005 Indian Standard MELAMINE (2, 4, 6 TRIAMINO 1, 3, 5 TRIAZINE ) — SPECIFICATION 1 SCOPE the lotofconsignment ormanufacture to be traced back from records. This standard covers the requirements and methods of sampling and test for melamine. 4.2.1 BIS Certljication Marking 2 ‘REFERENCES The container mayalso bemarked with the Standard Mark. The following standards contain provisions, which through reference in the text, constitute provisions 4.2.1.1 The use of Standard Mark is governed by of this standard. At the time of publication, the the provisions of the Bureau of Indian Standards editions indicated were valid. All standards are Act, 1986 and the Rules and Regulations made subject to revision and parties to agreements based thereunder. The details of conditions under which on this standard are encouraged to investigate the the licence for the use of the Standard Mark maybe possibility of applying the -most recent editions of granted to manufacturers or producers may be the standards indicated below: obtained from the Bureau of Indian Standards. IS No. Title 5 SAMPLING AND CRITERIA FOR CONFORMITY 265:1993 Hydrochloric acid (Jourth revision) Representative samples ofthematerial shall bedrawn 1070:1992 Reagent grade water(third revision ) and criteria for conformity of the material to the 4905:1968 Methods for random sampling requirement ofthis specification shall be determined according to the procedure prescribed inAnnex H. 8768:2000 Method ofmeasurement ofcolour in liquid chemical products platinum- 6 TESTS cobalt scale (second revision ) 6.1 Tests shall be carried out as given in CQI4 of Table 1. 3 REQUIREMENTS 6.2 Quality of Reagents 3.1 Description The material shallbe inthe form ofa whitecrystalline Unless-specified otherwise, A.R.Grade chemicals and powder and free from foreign impu r ities. distilled water shall be used in tests. Table 1 Requirements for Melamine (2,4,6 3.2 The material shall also comply with the Triamino 1,3,5 Triazine ) requirements given inTable 1when tested according (Clause 3.2) to the methods given inCOI4 of Table 1. 4 PACKING AND MARKING sl Characteristics Requirements Method of No. Test, Ref to 4.1 Packin_g Annex (1) (2) (3) (4) The material shall be packed in suitable packing media (multi-wall craft paper bag )or containers as i) Appearance White crystalline A agreed to between the purchaser and the supplier. powder, free from foreign impurities 4.2 Marking ii) Assay percent. 99.8 B .&fin The container shall be marked with the following 0.1 c iii) Losson drying. information: percent. Max 0.01 a) Name ofthe material; iv) Ash content. D percent. A4a.x b) Manufacturer’s name, initials ortrade-mark, v) pH 7.0-8.5 E if any; vi) Colour, APHA, 20 F c) Date/month of manufacture; Max d) Net mass of material; and vii) Clarity Clear to slight G turbid e) Identification incode orotherwise toenable 1 1S 15623: “2005 ANNEX A [ Table 1, S1No. (i) ] DETERMINATION OF APPEARANCE A-1 SCOPE A-2 PROCEDURE The method covers visual inspection ofmelamine. Place approximately 50gmelamine onaclean white paper of21 cm x 30 cm size. Visually examine and report the colour and impurities. ANNEX B [ Table 1,S1No. (ii) ] DETERMINATION OF ASSAY/PURITY B-1 SCOPE B-4.2 Inanother250mlbeaker,take300mgofcyanuric acid, add 100mldistilled water andwarmtill cyanuric The method covers the gravimetric procedure to acid gets dissolved. Add this hot .cyanuric acid determine purity ofmelamine. solution tomelamine solution. Heat the mixture just B-2 APPARATUS below boiling. Cool to the room temperature. Melamine-cyanurate w-illget precipitated. Allow it B-2. 1 Beaker, 500 ml. to stand for 2 h. Filter the precipitate through previously dried and weighed G-4 sintered glass B-2.2 Glass Rod crucible and transfers the precipitate quantitatively B-2.3 Sintered Glass Crucible G-4 into crucible using washing liquid. Finally wash the precipitate with minimum amount of distilled water. B-2.4 Analytical Balance, accuracy +0.0001 g. Take care that the total washing should not exceed B-2.5 Oven 25ml. Drythecrucible for 1hat 105”Cinhotairoven. Cool theG-4 crucible indesiccator, weigh and finally B-2.6 Hot Plate determine the weight of melamine-cyanurate. ‘B-2.7 Desiccators B-5 CALCULATION B-3 REAGENTS M*XO.4942 x 100 “Melamine,percent bymass = B-3. 1 Cyan uric Acid GR Ml B-3.2 Washing Liquid, 0.3 gcyanuric acid/litre. where B-4 PROCEDURE Ml = mass of the sample, and A4z= mass of melamine-cyanurate precipitate. B-4.1 Weighaccurately about 200 mgofsample and transfer it to 500-ml beaker. Add about 300 ml of NOTE—0,4942 is a factorfor converting mass of distilled water and heat until sample isdissolved. melamine-cyanurate to mass of melamine. 2 IS 15623:2005 ANNEX C [ Table 1,S1No. (iii) ] DETERMINATION OF LOSS ON DRYING C-1 SCOPE C-2.4 Analytical Balance, accuracy +0.0001 g. The method covers the analytical procedure to C-3 PROCEDURE determine moisture content by drying the sample in Weigh accurately about 10 g sample in a weighing oven at 105‘C. bottle. Dry itinthe oven at 105+2°C for 3h. Cool it C-2 APPARATUS in desiccator and weigh it. C-2. 1 Weighing Bottle with Stopper C-4 CALCULATION C-2.2 Desiccator Loss on drying, Loss inmass x 100 pcercent by mass = C-2.3 Oven Mass of sample ANNEX D [ Table 1,S1No. (iv) ] DETERMINATION OF ASHCONTENT D-1 SCOPE D-2.7 Muffle Furnace The method covers the analytical procedure to D-3 PROCEDURE determine non-volatile matter ofmelamine byignition at800”C. Weigh accurately about 100g of sample and transfer itinto initialIyweighed silica dish. Ignite the content D-2 APPARATUS of the dish carefully on burner. After complete D-2.1 Silica Dish, 100ml. ignition, transfer the dish with content into muffle furnace having 800+2°C temperature and keep itfor D-2.2 Spatula about 1 h. Cool the dish to room temperature in desiccator. Weigh the dish on balance, D-2.3 Pair of Tongs with Platinum Tip D-2.4 Desiccator D-4 CALCULATION D-2.5 Burner Ash content, Mass of residue x 100 percent by mass = D-2.6 Analytical Balance, accuracy +0.0001 g. Mass of sample IS 15623:2005 ANNEX E [ Table 1, S1No. (v) ] DETERMINATION OFpH ( 10PERCENT SUSPENSION ) E-1 SCOPE E-3 REAGENTS The method covers the analytical procedure to E-3.1 Distilled Water (see IS 1070 ). determine pH of 10 percent suspension-of melamine E-3.2 N/.100HCI inneutral distilled water. E-3.3 N/100 NaOH E-2 A-PPARATUS E-4 PROCEDURE E-2.1 pH Meter with Electrode Take100mlofdistilledwaterin250mlbeaker.Measure E-2.2 Beaker, 250 ml. thepH ofthe water. Adjust thepH of the water to 7.0 byeither adding N/100hydrochloric acid or sodium E-2.3 Magnetic Stirrer hydroxide. Add 10+ 0.1gmelamine rnto the 250 ml beaker and stir the suspension. After 3 rein, check E-2.4 Top Pan Batance, accuracy+ 0.01 g. thepH ofsuspension, till constant to one decimal and E-2.5 Stirring Bar report. ANNEX F [ Table 1,S1No. (vi) ] DETERMINATION OF COLOUR (APHA) F-1 SCOPE F-3:2 Cobalt Chloride Hexahydrate (CoC126H20 ) Themethodcovers theanalytical procedure tovisually F-3.3 Hydrochloric Acid (see IS265) determine the colour ( APHA ) of melamine F-3.4 Formaldehyde formaldehyde resin/solution by its comparison with the standard APHA solutions. F-4 PROCEDUR-E F-2 APPARATUS F-4.1 Preparation of Solution ‘F-2.1 Calorimetry Tbbes, 100ml. Transfer 50gofmelamine into 250 ml conical flask. Add 86 mlof formaldehyde solution. Heat iton hot F-2.2 Volumetric Flask, 250 and500ml. plate to 85 + 1‘C. Stir the suspension on magnetic F-2.3 Burette, 50 ml. stirrer for about 3min. F-2.4 Spectrophotometer F-4.2 Taking 50 mlofthe solution inF-4.1 carry out thetest asprescribed in1S8768. Compare the colour F-3 REAGENTS of melamine formaldehyde solution with standard F-3.1 Potassium Hexachloroplatinate( K2-PtCIJ platinum-cobalt standards and report. IS 15623:2005 ANNEX G [ Table 1,S1No. (vii) ] DETERMINATION OF CLARITY G-1 SCOPE G-4 PROCEDURE Themethodcoverstheanalyticalprocedure forvisually G-4.1 Preparation ofStandard Turbidity Solution determining clarity ofmelamine formaldehyde (MF) G-4.1.1 Base So/ution I resin prepared by dissolving specified quantity of melamine informaldehyde solution (Formaldehyde: Take 25 ml of hydrazine sulfate solution into 25 ml Melamine3:1mol/molratio)atincreasedtemperature, hexamine solution the mixture iskept for 24 h. The after specified period by comparison with standard resulting suspension is kept for 2 months. turbidity solution. G-4.1.2Base Solution 2 G-2 APPARATUS Fromtheabovesolutiontake 15mlsolutionandtransfer G-2.1 Conical Flask, 250 ml. itin 1000 mlvolumetric flask. Dilute itwith distilled water tothe mark. G-2.2 Calorimetric Tbbe G-2.3 Thermometer, 0° C-1100C. G-4.1.3 Turbidity Standards G-2.4 Hot Plate Turbidity standards are as under: G-2.5 Oven a) OmIBase2solution + 100mldistilled water: Clear ‘G-2.6 Top Loading Balance, accuracy * 0.01 g. b) 5 mlBase2solution + 95mldistilled water: G-2.7 Measuring C-ylinder Almost Clear G-2.8 Volumetric Flask, 1000 ml. c) 10mlBase2solution+ 90mldistilledwater: Slight Turbid G-2.9 Magnetic Stirrer with Hot Plate d) 20mlBase2solution+ 80mldistilled water: G-2.1O Pipette, 100 ml. Turbid G-2.11 Pipette (Graduated), 10ml. NOTE — The standard solution’s stability can last for about2weeks. G-2.12 Magnet Bar G-4.2 Resin Preparation for Turbidity Check G-3 ‘REA-GENTS Transfer 50gofmelamine into 250 ml conical flask. G-3.1 Formaldehyde, having concentration Add 86 ml of formaldehyde solution. Heat it on hot 36.0 percent, Min. plateto85+ I“C.Stirthesuspensiononmagneticstirrer for about 3min. G-3.2 Turbidity Standard G-5 OBSERVATION G-3.2. 1 Hydrazine Sulphate, 0.5 ghydrazine sulfate in50mldistilled water keep this solution for 5to6h. Atler additional 2mincompareturbidity ofmelamine formaldehyde solution with the standard turbidity G-3.2.2 Hexamine, 2.5 gofhexaminein25mldistilled water. solutions and report the observation.