MELAMINE DETAILED REQUIREMENTS - see Table 1 Table Melamine content, at least % 99,8 99,6. 2. Ash content, not more than % 0,02 0,03

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1 1. SUBJECT OF THE SPECIFICATION The subject of this Technical Specification is elaine anufactured by theral decoposition of urea. The cheical forula is C 3H 6N 6. Two grades of elaine are anufactured, designated by sybols A1 and A2. 2. REQUIREMENTS 2.1. GENERAL REQUIREMENTS Melaine is white crystalline powder without visible echanical ipurities DETAILED REQUIREMENTS - see Table 1 Table 1 No. Requireents Unit A1 Grade A2 1. Melaine content, at least % 99,8 99,6 2. Ash content, not ore than % 0,02 0,03 3. Moisture content, not ore than % 0,1 0,1 4. Reactivity, at least inutes Color of elaine-foraldehyde resin, not ore than Pt-Co (1) 6. Iron content, not ore than pp ph range of 2% elaine solution in water - 7,5-8,5 7,5-8,5 8. Clarity of elaine-foraldehyde solution - clear or alost clear alost clear or slightly turbid 9. Color of elaine-foraldehyde solution, not ore than Pt-Co (1) (1) The color ay slightly differ fro the Pt-Co standard scale 3. LABELLING Product label shall be located in conspicuous location and shall be peranently affixed to the packing. Label text and inforation should be in a size of type large enough to be readily legible. Labelling ust ention: the nae, address, telephone nuber and logo of the anufacturer the nae of the product: MELAMINE the noinal quantity of the product the batch nuber Handling sybols: Keep dry It is allowed to apply other printed inforation on the packing, provided that it has been agreed with the custoer. 4. PACKING Melaine shall be packed as follows: 25kg vented paper bags, to be laid loosely or on wooden pallets; the palleted bags should be protected by wrapping with theral shrink foil Grupa Azoty Zakłady Azotowe Puławy S.A. Page 1 of 9

2 polypropylene big-bags of kg capacity bulk in tank vehicles or tank wagons on request, in custoer s packing 5. STORAGE Melaine should be stored in clean, well ventilated roofed facilities while providing protection against oisture and dirt. Product ust be kept away fro incopatibles such as oxidizing agents, acids. Iproper storage ay affect product quality. 6. TRANSPORT Melaine shall be transported in any roofed eans of transport and protected fro oisture. ADR/RID regulations do not apply to this product. 7. ANALYTICAL METHODS 7.1. TESTING SCHEDULE see Table 2 No. Test description Liits as per: Test description as per: Table 2 1. Deterination of Melaine content Deterination of ash content Deterination of oisture content Deterination of reactivity Deterination of color of elaine-foraldehyde resin Deterination of iron content Deterination of ph of 2% elaine solution in water Deterination of clarity of elaine-foraldehyde solution Deterination of color of elaine-foraldehyde solution LOT QUANTITY Each batch shall contain not ore than 100 tons of elaine SAMPLING Melaine is a hoogenous product. Sapling fro a batch is carried out during packaging, with the use of autoatic saplers. Fro a priary saple, a final bulk saple of approx. 1.5kg is prepared. The final bulk saple is split into two parts: one for testing and the other one for archiving purposes. In case of anual sapling, PN-ISO-8213:1999 guidelines shall be applied CHECKING FOR COMPLIANCE WITH GENERAL REQUIREMENTS Check visually for copliance with general requireents DETERMINATION OF MELAMINE CONTENT BY POTENTIOMERIC TITRATION WITH SULPHURIC ACID Principle of the ethod. Melaine is a weak base. One ol of elaine reacts with 1 ol of acid. This allows to easure elaine Grupa Azoty Zakłady Azotowe Puławy S.A. Page 2 of 9

3 purity by potentioetric titration with 0.5 N sulfuric acid Apparatus and reagents. a) Metroh potentioetric titrator (procedure MET ph) b) Cobined ph-etric electrode c) l beaker d) 0.5N standard solution of sulphuric acid Deterination procedure. Weigh a 1,2-1,3 g test saple of elaine with an accuracy of ±0.0001g in a 200 l beaker. Add 100 l of distilled water and place the beaker on a hot plate agnetic stirrer. Apply heat while intensely stirring until elaine dissolves copletely (do not allow the solution to boil). Iediately after dissolution transfer the test saple to the titrator, do not ierse the electrode and start the elaine titration procedure. After adding l of 0.5N sulfuric acid (the aount of the acid added depends on acid factor value) titration is interrupted for 30 inutes, during which tie the solution is intensely stirred and cooled to 25 C. Then ierse the e lectrode and continue titration by adding very sall aounts of the acid (V step-0.05 l, titr rate 1 l/in) until equivalence point EP1 is reached, where second derivative of ph/v is equal to zero. The tie necessary to coplete this analysis is approx. 50 inutes Calculation and deterination of results. Calculate the Melaine content (X) as weight percentage (w/w) using the following forula: where: V F 0, % Melaine = V volue (l) of 0,5N H 2SO 4 used to deterine equivalence point EP1 F factor of 0,5N H 2SO 4 standard solution weight (g) of elaine test saple 0,06307 aount (g) of elaine which equals to 1l of H 2SO Final result of deterination. The final results should be an arithetic ean of the results of at least two consecutive tests, which differ fro each other by not ore than 0,1% (w/w) DETERMINATION OF ASH CONTENT Principle of the ethod. The ethod consists in deterination of ash (residue on ignition) after incineration of a elaine saple followed by heating at 900 C Deterination procedure. Weigh g of elaine in a quartz crucible previously heated at 900 C to a constant ass and weigh ed on an analytical balance with an accuracy of 0,0002 g. Put the crucible with elaine into a uffle furnace. Heat up quickly to 350 C, then increase the teperature slowly to 900 C. Heat at that teperature until the saple is copletely incinerated (approxiately 60 inutes). Next, place the crucible into a desiccator and weigh it with an accuracy of 0,0002 g Calculation and deterination of results. Calculate the ash content (X) as weight percentage (w/w) using the following forula: Grupa Azoty Zakłady Azotowe Puławy S.A. Page 3 of 9

4 where: X = weight (g) of elaine test saple 1 weight (g) of the ash (residue on ignition) Final result of deterination. The final results should be an arithetic ean of the results of at least two consecutive tests, which differ fro each other by not ore than 0,001% (w/w) DETERMINATION OF MOSITURE CONTENT Principle of the ethod. The ethod consists in drying of known aount of elaine at C until a constant ass is obtain ed Deterination procedure. Dry a weighing bottle of diaeter at C to a constant ass, allow to cool it in a desi ccator and weigh it with an accuracy of 0,0002 g. Weigh 10 g of elaine with the sae accuracy into the weighing bottle and place it in a drying oven. Dry under above prescribed conditions to a constant ass. Allow the weighing bottle to cool down in a desiccator, then weigh it with an accuracy of 0,0002 g Calculation and deterination of results. Calculate the oisture content (X) as weight percentage (w/w) using the following forula: where: weight (g) of elaine test saple 1 loss on drying (g) X = Final result of deterination. The final results should be an arithetic ean of the results of at least two consecutive tests, which differ fro each other by not ore than 0,01% (w/w) DETERMINATION OF REACTIVITY Principle of the ethod. The ethod consists in easuring the tie needed to attain coplete resinification of elaine with foraldehyde Instruent and apparatus. a) ph-eter b) two-neck round-bottoed flask of 500 l c) agnetic stirrer with glycerin seal d) reflux condenser e) tier f) water bath Grupa Azoty Zakłady Azotowe Puławy S.A. Page 4 of 9

5 g) 100 l beaker Reagents and solutions. a) Foralin, a 37±0.5% solution containing 4-6% of ethanol; neutralized with sodiu hydroxide solution to ph=8.5±0.1, easured by a ph-eter. The foralin ust not contain any polyers of foraldehyde. The color of the foralin shall be ax 5 according to Pt-Co scale. b) Sodiu hydroxide, analytical grade, solution of c=0,1 ol/l Deterination procedure. Weigh 60 g of elaine with an accuracy of 0,1 g into a two-neck flask and add 110 l of foralin. Connect the flask with a reflux condenser and a stirrer. Ierse the flask in a boiling water bath aking sure that at least ¾ of the flask is suberged and at the sae tie start the stirrer and record the tie. After 35 inutes, take with a pipette 5 l of the solution into a dry 100 l beaker and allow it to cool down to 25 C. Put a piece of white paper under the beaker, with two crossing lines of 1- thickness plotted in ink on the paper. Next, titrate the saple with distilled water having teperature of 25 C unt il peranent turbidity is obtained and the lines on the paper are no longer visible. Repeat the titration every 5 inutes until the total aount of water used for the deterination is 20 l. Reactivity of elaine corresponds to the tie needed to coplete titration by using 20l of water Final result of deterination. The final results should be an arithetic ean of the results of at least two consecutive tests, which differ fro each other by not ore than 5 inutes DETERMINATION OF COLOR OF MELAMINE-FORMALDEHYDE RESIN Principle of the ethod. The deterination consists in coparing the color of a test saple with Pt-Co standards Reagents and solutions. Platinu-Cobalt standards ade according to PN-EN ISO : Deterination procedure. After carrying out the reactivity test, pour the resin (filter if turbid) to a pre-heated Nessler cylinder and deterine the color according to PN-EN ISO :2006. The result shall be given according to the requireents of PN-EN ISO : DETERMINATION OF IRON CONTENT Principle of the ethod. The ethod consists in the foration of red coplex salts by reacting iron salts and 2,2 -dipyridyl. Iron content is found by spectrophotoetric easureent of absorbance of the coplex fored and reading the concentration of iron fro a standard curve Instruents. Spectrophotoeter or photocolorieter with a 522 n wavelength filter and a 5-c cell Reagents and solutions. Grupa Azoty Zakłady Azotowe Puławy S.A. Page 5 of 9

6 a) Ferrous aoniu sulfate Fe(NH 4) 2(SO 4) 2 6H 2O b) Hydroxylaine hydrochloride, analytical grade; solution prepared as follows: weigh 10 g of Hydroxylaine hydrochloride into a 100 l voluetric flask, dissolve in distilled water and dilute to volue with the sae solvent. c) 2,2 -dipirydyl, analytical grade; solution prepared as follows: weigh 1 g of 2,2 -dipirydyl into a 100 l voluetric flask, dissolve in 98% ethyl alcohol and dilute to volue with the sae solvent. d) Sulphuric acid, analytical grade; prepare aqueous solution of 1:1 (v/v) e) Aoniu acetate, analytical grade; solution prepared as follows: weigh 200 g of aoniu acetate into a 1000 l voluetric flask, dissolve in distilled water and dilute to volue with the sae solvent. f) Potassiu pyrosulfate, analytical grade g) Basic standard iron solution prepared as follows: weigh accurately 0,702 g of ferrous aoniu sulfate into a 1000l voluetric flask, add 200l of distilled water and 4l of concentrated sulfuric acid. Dilute to volue with distilled water and shake well. 1 l of this solution contains 0,1 g Fe. h) Reference standard iron solution prepared as follows: Transfer 20 l of the basic standard iron solution and 2 l of sulphuric acid solution (1:1) into a 1000 l voluetric flask. Dilute to volue with distilled water and ix well. 1 l of this solution contains 0,002 g Fe. Solution ust be freshly prepared on the day of standard curve deterination. i) Aonia water, analytical grade; 10% solution of aonia in water Preparation of standard curve Weigh 2 g of potassiu pyrosulfate into seven 100 l voluetric flasks. Add to each flask 2 l of aqueous sulfuric acid solution, 20 l of distilled water and specified volue of reference standard iron solution given in Table 3. Flask No Volue of reference standard solution, l 0, Corresponding aount of Fe, g 0,0 0,01 0,02 0,03 0,04 0,05 0,06 Table 3 Next, transfer to each flask 5 l of hydroxylaine hydrochloride solution, 10 l of aoniu acetate solution, 10 l of aonia water, and 1 l of 2,2 -dipyridyl solution, dilute to volue with distilled water and ix. After 30 inutes, easure absorbance of the reference solutions thus prepared on a spectrophotoeter or a photocolorieter against a parallel prepared blank (flask no. 1) at 522 n wavelength, using cells of 5 c thickness. Plot a standard curve based on the results obtained, with iron concentration in g/100 l on Y-axis and the corresponding absorbances on X axis Deterination procedure. Melt the residue on ignition (ash) fro the test carried out according to paragraph above with 2 g of potassiu pyrosulfate. Allow the elt to cool down, then dissolve it by heating in an evaporating dish with 2 l of sulfuric acid solution and 20 l of distilled water. Subsequently, transfer the content quantitatively into a 100 l voluetric flask. Next, add 5 l of hydroxylaine hydrochloride solution, 10 l of aoniu acetate solution, 10 l of aonia water, 1 l of 2,2 -dipyridyl solution to the flask, dilute to volue with distilled water and ix. After 30 inutes, easure absorbance using the sae conditions as when aking the standard curve. Fro the standard curve, read iron concentration in g/100 l of solution, corresponding to the easured absorbance Calculation and deterination of results. Calculate the iron content (X) in pp using the following forula: Grupa Azoty Zakłady Azotowe Puławy S.A. Page 6 of 9

7 where: X = iron content (g/100l of solution) read fro the standard curve 1 weigh (g) of elaine saple according to Final result of deterination. The final results should be an arithetic ean of the results of at least two consecutive tests, which differ fro each other by not ore than 0,2 pp DETERMINATION OF ph of 2% AQUEOUS SOLUTION OF MELAMINE Deterination procedure. Weigh 2 g of elaine with an accuracy of 0.1 g into a 300 l beaker. Transfer 100 l of fresh hot distilled water into a beaker and dissolve elaine while stirring for 15 inutes. After decanting, easure ph of the solution at C with an accuracy of 0,1 using a ph-eter DETERMINATION OF CLARITY OF MELAMINE-FORMALDEHYDE SOLUTION Principle of the ethod. Melaine can contain coponents which are insoluble in foralin solution. Those coponents becoe visible when a certain aount of elaine (foraldehyde/elaine olar ratio of 3:1) is dissolved in water at 80 C. The turbidity caused by those coponents is copared with that of turbidity reference standards Reagents and solutions. a) Foralin having the following coposition: - foraldehyde 36-37% - foric acid ax 0,03% - ethyl alcohol ax 5% - color ax 5 Pt-Co b) Color reference standard solutions according to PN-EN ISO :2006 c) Turbidity reference standard solutions prepared according to Preparation of turbidity standards. A ilk-white slurry of a polyer called forazine is used for the preparation of turbidity standards. Preparation of basic standard solution: a) Dissolve 1,000 g of hydrazine sulfate (NH 2) 2 H 2SO 4 in distilled water and dilute to volue in a 100 l voluetric flask. b) Dissolve 10,000 g of hexaethylenetetraine (CH 2) 6N 4 (urotropine) in distilled water and dilute to volue in a 100 l voluetric flask. c) Transfer 5.0 l of each solution thus prepared into a 100 l voluetric flask, ix and leave for 24 hours at 25 ±3 C. The teperature is essential for the proper foration of the polyer. After 24 hours Grupa Azoty Zakłady Azotowe Puławy S.A. Page 7 of 9

8 dilute to volue and shake well. The turbidity of the obtained basic solution is 400 FTU. Its durability is axiu 1 onth. Preparation of working standard solution: Transfer 25 l of the basic solution into a 100 l voluetric flask and dilute to volue with distilled water. The turbidity of the obtained solution is 100 FTU. Preparation of reference standard solutions: Place, respectively, 2, 5 and 10 l of the 100 FTU solution into three separate 100 l beakers. Dilute to volue with distilled water, add 1 drop of saturated ercury chloride solution in order to fix the solution and ix. Transfer the reference standard solutions into 250 l Erlenayer flasks and plug the flasks. Durability of the reference standard solutions is 2 weeks. Reference standard solution Evaluation scale 2 FTU reference solution clear 5 FTU reference solution alost clear 10 FTU reference solution slightly turbid Deterination procedure. Weigh 50±0.1 g of elaine into a 250 l conical flask, add 86 l of foralin solution (with elaine/foralin olar ratio of 1:3). Place a agnetic stirring bar inside the flask. Place the flask on the hot plate agnetic stirrer and heat, while stirring continuously, up to 80 C d uring 5 inutes. Reove the flask fro the hot plate and after about 2 inutes, carry out visual evaluation of the solution clarity Evaluation of solution clarity. Copare the solution tested with turbidity reference standards. The evaluation should be carried out in daylight, while holding the Erleneyer flasks at eye level. Shake the standards before the evaluation. Clear solution: turbidity of the saple is lower than 2 FTU standard. Alost clear solution: turbidity of the saple is higher than 2 FTU and lower than 5 FTU standard. Slightly turbid solution: turbidity of the saple is higher than 5 FTU and lower than 10 FTU standard DETERMINATION OF COLOR OF MELAMINE-FORMALDEHYDE SOLUTION After deterining the turbidity of a elaine-foraldehyde solution (filter if turbid), pour the solution into a preheated Nessler cylinder and deterine the color according to PN-EN ISO :2006. The final result should be given according to PN-EN ISO : RESULTS EVALUATION AND TEST CERTIFICATE. A elaine batch shall be considered to eet the requireents of this Technical Specification if test results confor with the requireents indicated in Table 1. The anufacturer is obliged to send to the custoer a certificate stating the copliance of the product with the requireents of this Technical Specification. 7. REFERENCES Grupa Azoty Zakłady Azotowe Puławy S.A. Page 8 of 9

9 PN-ISO 8213: Cheical products for industrial use. Sapling techniques. Solid cheical products in the for of particles varying fro powders to coarse lups. PN-EN ISO :2006 Clear liquids Estiation of colour evaluation by the platinu-cobalt scale Part 1: Visual ethod. 8. ADDITIONAL INFORMATION supersedes WT-2012/ZA-7 Grupa Azoty Zakłady Azotowe Puławy S.A. Page 9 of 9