FC20004 TECHNICAL SPECIFICATION No. 5 PRILLED NPK COMPLEX CHEMICAL FERTILIZERS NPK and NP complex chemical fertilizers are mixtures of monoconstituent inorganic substances: ammonium phosphate, calcium phosphate, and ammonium nitrate. NPK sorts also contain potassium chloride (or potassium sulphate). 1.Identification and classification Name: NPK or NP complex fertilizers Chemical formula: EC Number: CAS Number: Molecular mass: ECHA Registration Number for ammonium nitrate: 012119490981270064 EC Number: 2293478 CAS Number: 6484522 ECHA Registration Number for monoammonium phosphate: 012119488166290047 EC Number: 2317645 CAS Number: 7722761 ECHA Registration Number for diammonium phosphate: 012119490974220044 EC Number: 2319878 CAS Number: 7783280 ECHA Registration Number for dicalcic phosphate: 012119490064410017 EC Number: 2318261 CAS Number: 7757939 ECHA Registration Number for calcium carbonate: 012119486795180070 EC Number: 2074399 CAS Number: 471341 ECHA Registration Number for potassium chloride: excepted from registration EC Number: 2312118 CAS Number: 7447407 ECHA Registration Number for potassium sulphate: 012119489441340029 EC Number: 2319155 CAS Number: 7778805 NPK and NP complex fertilizers are not classified as dangerous mixtures according to Directive 1999/45/EC and to Regulation (EC) No. 1272/2008. 2. Technical quality conditions: see the Annex Observations: at the client s request, additional tests may be performed or other requirements may be established. The test results for the following: TotalN, Total P 2 O 5, AmmoniaN, NitricN, K 2 O soluble in water, P 2 O 5 soluble in citric acid, P 2 O 5 neutral ammonium citrate, P 2 O 5 soluble in water, CaO, MgO, SO 3 soluble in water, Zn, B, Cl, total combustible materials, ph, are guaranteed by the producer and their determinations are performed upon request. Date of issue: 23.02.2015 Version: 22 Page: 1 / 10
3. Testing methods Appearance: visual Total Nitrogen: determined according to SR ISO 5315:1994 respectively SR EN 15476:2009. The testing method is applied for the dosing of the ammonia and the nitric nitrogen from the fertilizers, by reduction (total nitrogen) with Dewarda. The nitrates are reduced to ammonia with Dewarda alloy in an alkaline environment. The formed ammonia is captured by entrainment with water vapours, in a known quantity of sulphuric acid, and the excess of sulphuric acid is titrated with sodium hydroxide. AmmoniaN: is determined according to SR ISO 5314:1994, respectively SR EN 15475:2009. The testing method consists in displacing the ammonia by an excess of sodium hydroxide, entrainment with water vapours, capturing the quantity of ammonia in a standard volume of sulphuric acid and titration of the sulphuric acid excess using a standard solution of sodium or potassium hydroxide. NitricN: is determined by calculation. Total P 2 O 5 : according to SR ISO 7497:1997, SR ISO 6598:1996, respectively SR EN 15956:2011 for extraction and SR EN 15959:2011 for determination. After a possible hydrolysis, the phosphorus is precipitated in an acid environment as quinoline phosphomolybdate. After filtering and washing, the precipitate is dried at 250 C and then weighted. P 2 O 5 soluble in water: SR ISO 5316:1996, SR ISO 6598:1996, respectively SR EN 15958:2011 for extraction and SR EN 15959:2011 for determination. Phosphorous extraction in water by stirring the sample in determined conditions. After a possible hydrolysis, the phosphorus is precipitated in an acid environment as quinoline phosphomolybdate. After filtering and washing, the precipitate is dried at 250 C and then weighted. P 2 O 5 soluble in neutral ammonium citrate: according to SR 114112:1198, method 6.3, respectively SR EN 15957:2011 for extraction and SR EN 15959:2011 for determination. Phosphorous extraction at a temperature of 65 C using a neutral ammonium citrate solution (ph = 7) in specific conditions. After a possible hydrolysis, the phosphorus is precipitated in an acid environment as quinoline phosphomolybdate. After filtering and washing, the precipitate is dried at 250 C and then weighted. K 2 O soluble in water: according to SR ISO 5317:1997 for extraction in water, SR ISO 5318:1997 for determination, respectively SR EN 15477:2009. The potassium from the sample to be analyzed is dissolved in water. After eliminating or fixing the substances that can interfere (ammonium ion interference) in the quantitative determination using a sodium salt of the ethylene diamide tetraacetic acid (EDTA) and formaldehyde, the potassium is precipitated in a slightly alkaline environment, as potassium tetraphenylborate. Moisture/water content: according to SR EN 134661:2002 The method consists in extracting the water from fertilizers using methanol and titration with a standardized Karl Fischer reagent titration of a known quantity of water. Granulation: according to STAS 1301891 section 4.3., respectively SR ISO 25911:1998. The sample to be tested is mechanically or manually sieved on a group of sieves with the mesh size of 1; 4 mm. The mass placed on each sieve and the mass passing through the last sieve of the kit is weighted and then the percentage of material that passes through the sieves is calculated. ph: according to STAS 8619/390. Date of issue: 23.02.2015 Version: 22 Page: 2 / 10
The determination is performed using a laboratory phmeter in a solution obtained from 10 g of product and 100 ml of distilled water. Combustible components: according to Regulation (EC) No. 2003/2003, Annex III, method 3. The method consists in the following: in the first stage, the carbon dioxide produced by the inorganic fillings is removed using an acid. The organic components are oxidised with a mixture of chromic acid and sulphuric acid. The carbon dioxide is absorbed in a solution of barium hydroxide. The precipitate is dissolved in a solution of hydrochloric acid and it is measured by retitration with a solution of NaOH. Calcium: according to standard SR EN 15961:2012 for the extraction of the sorts soluble in water and SR EN 15960:2012 for the extraction of total calcium; SR EN 16196:2013 for determination. Precipitation of calcium contained in a portion of the extract solution in the form of an oxalate, which is determined by titration using potassium permanganate. It is a secondary nutrient and the content is declared only if it is present in a quantity of at least 2 of the calcium oxide CaO, according to Regulation (EC) No. 2003/2003. Magnesium: soluble in water according to standard SR EN 15961:2012 for extraction and SR EN 16196:2013 for determination. Determination of magnesium by atomic emission spectroscopy. It is a secondary nutrient and the content is declared only if it is present in a quantity of at least 2 of the magnesium oxide MgO, according to Regulation (EC) No. 2003/2003. Sulphur: soluble in water according to standard SR EN 15961:2012 for extraction and SR EN 15749:2010 for determination. Sulphates from chemical fertilizers are determined using the gravimetric method as barium sulphate. It is a secondary nutrient and the content is declared only if it is present in a quantity of at least 5 of the sulfur trioxide SO 3 according to Regulation (EC) No. 2003/2003. Zinc: according to Regulation (EC) No. 2003/2003 method 9.1 and 9.11. Extraction from fertilizers by dissolution in HCl diluted by boiling. Determination of zinc is made by atomic emission spectroscopy. It is a microelement and the content is declared if it is present in a minimum quantity, according to Regulation (EC) No. 2003/2003. Boron: according to Regulation (EC) No. 2003/2003 method 9.1 and 9.11. Extraction from fertilizers by dissolution in HCl diluted by boiling for the determination of microelements content of which is less than 10. Determination of boron is accomplished by Atomic emission spectroscopy. Represents a trace element and content provided is declared to be present in minimum quantity under Regulation (EC) no. 2003/2003 Chlorides: are determined according to standard SR EN 16195:2013. The method is used for producing complex fertilizers with potassium sulphate. Chlorides dissolved in water are precipitated in an acid environment using a silver nitrate standard solution in excess. The excess is titrated using an ammonium thiocyanate solution in the presence of ferric ammonium sulphate (Volhard method). 4. Quality control Quality control is performed on batches of max. 300 tons. Each delivery is accompanied by the Conformity Statement. At the client s request, the product is accompanied by a Test Report, and, when expressly requested, by an estimative calculation of the extended incertitude of the test result. Date of issue: 23.02.2015 Version: 22 Page: 3 / 10
5. Tolerances According to Regulation (EC) No. 2003/2003 Annex II; tolerances are negative values in mass percentage. Inorganic fertilizers with primary nutrients N 1.1 P 2 O 5 1.1 K 2 O 1.1 P 2 O 5 soluble in citric acid, formic acid, soluble in neutral ammonium citrate, in alkaline ammonium citrate and in water. Tolerances admitted for the declared content of various forms of nitrogen or for the declared solubility of the phosphorus pentoxide are one tenth of the total content in the corresponding element, with maximum 2 mass percentage, considering that the total nutrient content fits within the limits stipulated in Annex I and is in accordance with the above mentioned tolerances. Binary fertilizers 1.5 The nutrient concentrations sum of N+P 2 O 5 should not exceed the above tolerance in respect to the declared value. Tertiary fertilizers 1.9 The nutrient concentrations sum of N+P 2 O 5 +K 2 O should not exceed the above tolerance in respect to the declared value. Secondary nutrients in fertilizers Admitted tolerances for the declared value of Ca, Na and S must be a quarter of the declared value of these nutrients, up to maximum 0.9 in absolute terms for CaO, MgO, Na 2 O and SO 3 (e,g, 0.64 for Ca, 0.55 for Mg, 0.67 for Na and 0.36 for S). Micronutrients in fertilizers The tolerance in relation to the declared content of micronutrients has to be: 0.4 in absolute terms for a content over 2 a fifth of the declared value for a content of maximum 2 6. Packaging The product is packed in polyethylene bags or double bags (polyethylene and polypropylene). The polyethylene bags are closed by welding, and the polypropylene bags are closed by sewing. Usually, the product is packed in 50 kg bags, but it can also be packed in 40 kg, 500 kg, 600 kg or 1000 kg bags or it may also be delivered in bulk. The marking on the bags is in accordance with the current regulations. Product name: complex fertilizer Declared content for each nutrient: TOTAL NITROGEN N, AMMONIAN, NITRATE N, TOTAL P 2 O 5, P 2 O 5 SOLUBLE IN WATER, P 2 O 5 SOLUBLE IN NEUTRAL AMMONIUM CITRATE, K 2 O SOLUBLE IN WATER, expressed in mass percentage in the form of a whole number The nutrients have to be declared both in words and chemical symbols, e.g. Nitrogen (N) Net weight of the fertilizer Name and brand of the producer Name, commercial name or brand and address of the person responsible for trading the product, with headquarters in Romania or in the European Community (for export). The marking on the bags and the accompanying documents have to be provided in at least one official EU member states language (for export). Packed chemical products are identified through the information written on labels or on the package. The identification data for the products delivered in bulk or in packages that exceed 100 kg is mentioned on the accompanying documents. Date of issue: 23.02.2015 Version: 22 Page: 4 / 10
7. Handling, storage, transportation, guarantees The product should be stored in closed, dry, clean and well ventilated areas away from heat of and fire sources. Storage and transportation is performed in piles of maximum 10 rows for the 40 kg and 50 kg bags and 2 rows for the 500 kg, 600 kg and 1000 kg bags. Transportation means must be clean, dry and covered with waterproof covers, free of sharp edges that might cut or rip the bags. The product can also be transported in bulk, in wagons covered, with a waterproof, nonflammable cover, or in metallic TALS. a. For the NPK sorts: 2766; 2655; 26130; 2713.50 During transportation, the stipulations of the RID (European Agreement concerning the International Carriage of Dangerous Goods by Rail), ADR (European Agreement concerning the International Carriage of Dangerous Goods by Road) and IMDG (International Maritime Transportation Regulation concerning Dangerous Goods) need to be respected. The danger label to be placed on the transportation means is hazard label 5.1. According to ADR, RID or IMDG classification, these sorts of fertilizers have the material classification number UN 2067, class of danger 5.1, being classified as fertilizers containing ammonium nitrate. For bulk deliveries on sea, the ship s holds must be clean and dry (without any traces of oil, grease or residues from previous transports) and with no traces of loose rust on the walls; no paper should be applied on the walls of the holds. For sea transports, the fertilizer must pass the trough test. b. For NPK sorts: 20200; 21210; 22220; 131317; 141417; 151515; 161516; 16168; 161616; 16816; 16816+2Mg; 151015; 18818; 201010; 20717; 221111; 21712; 21713; 21714; 221010; 221010+0,04B+0,05Zn; 22612; 22612+3S+0.2B+0.2Zn; 20515; 21516; 25510; 25510+3S+0,02Mg; 2555; 25412 24510. No danger label needs to be placed on the means of transport. These are not subject to ADR, RID or IMDG. According to ADR, RID, IMDG classification, granulated NPK fertilizers are classified as fertilizers with ammonium nitrate, uniform mixtures of nitrogen/phosphate, nitrogen/potassium or nitrogen/phosphate/potassium, with not more than 70 ammonium nitrate and not more than 0.4 total combustible material, organic substances expressed in carbon equivalent or with not more than 45 ammonium nitrate irrespective of their content of combustible material, material classification number (UN) 2071. In case of bulk deliveries on sea, the ship s holds must be clean and dry (without any traces of oil, grease or residues from previous transports) and with no traces of loose rust on the walls; no paper should be applied on the walls of the holds. For sea transports, the fertilizer must pass the trough test. If the fertilizer passes the trough test, then it is not considered as dangerous for sea transport, except for air transport, were it remains classified under UN 2071. Term of validity: 12 months from the date of bagging for the product packed in bags 12 months for the bulk product from the date mentioned in the accompanying documents, in compliance with specified transport and storage conditions. Date of issue: 23.02.2015 Version: 22 Page: 5 / 10
8. Security measures People working with complex fertilizers for long periods of time (for example in storehouses) will use individual protection equipment: gloves and dust mask when necessary. In order to avoid the effects of the product on skin, washing is mandatory after handling the product. After emptying the polyethylene and polypropylene bags, these will not be used in household activities (packing and storing food etc.). In certain temperature conditions, in the presence of combustible substances (lubricants, diesel fuel, petroleum etc.), organic substances and of certain impurities (metal dust) as well as in the presence of direct sources of heat (flame), complex fertilizers may slowly decompose, in the entire quantity of fertilizer, releasing massive clouds of toxic gases. In this case, the affected area will be flooded with water. Call immediately the local Inspectorate for Emergency Situations. In case of incidents/accidents immediately notify the local Inspectorate for Emergency Situations. Further details in the compound substances Safety Data Sheet. NPK Plant Manager Quality Manager Technical Manager Eng. Iuliu SUCIU Eng. Camelia IANCULESCU Eng. Aurel BOTEZAN Date of issue: 23.02.2015 Version: 22 Page: 6 / 10
ANNEX TO THE NPK TECHNICAL SPECIFICATION No. 5 QUALITY CONDITIONS N in relation to dry substance P 2 O 5 in relation to dry substance Sort 20200 21210 22220 2713.50 26130 Appearance total 20 21 22 27 26 ammonia 11.3 11.8 12 14.4 13.9 nitric 8.7 9.2 10 12.6 12.1 total 20 21 22 13.5 12.16 soluble in water 12 12.6 13.2 8.1 7.8 soluble in neutral ammonium citrate 18 18.9 19.8 12.2 11.7 soluble in citric acid 2 19.6 20.5 21.5 13.2 12.7 Water content, max 0.6 0.6 0.6 0.6 0.6 Granulometry between 1 4 mm, min 95 95 95 95 95 below 1 and above 4 mm, max. 5 5 5 5 5 Total combustible materials, max 0.4 0.4 0.4 0.4 0.4 ph, min. 4.5 4.5 4.5 4.5 4.5 Date of issue: 23.02.2015 Version: 22 Page: 7 / 10
N in relation to dry substance P 2 O 5 in relation to dry substance K 2 O soluble in water in relation to dry substance Sort 131317 151515 161616 16816 151015 201010 221111 21713 22612 Appearance 221010 +0.04B+ 0.05Zn total 13 15 16 16 15 20 22 21 22 22 ammonia 7.3 8.3 8.8 8 8.1 11 11.8 11.4 11.4 11.8 nitric 5.7 6.7 7.2 8.5 6.9 9 10.2 9.6 10.6 10.2 total 13 15 16 8 10 10 11 7 6 10 soluble in water 7.8 9 9.6 4.8 6 6 6.6 4.2 3.6 6 soluble in neutral ammonium 11.7 13.5 14.4 7.2 9 9 9.9 6.3 5.4 9 citrate soluble in citric acid 2 12.7 14.7 15.6 7.8 9.8 9.8 10.7 69 5.9 9.8 from potassium chloride from potassium 17 15 16 16 15 10 11 13 12 10 sulphate Cl for the sorts with potassium sulphate, max 0.85 0.8 0.8 0.8 0.5 0.7 0.6 0.5 SO 3 soluble in water for the sorts with potassium sulphate, 14.5 12.8 13.6 13.6 12.8 8.5 9.4 11.1 10.2 8.5 Water content, max. 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 Granulometry between 1 4 mm, min. 95 95 95 95 95 95 95 95 95 95 below 1 and above 4 mm, max 5 5 5 5 5 5 5 5 5 5 Total combustible materials, max. 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 ph, min 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 Zn, from zinc sulphate B, from borax 0.05 0.04 MgO, Date of issue: 23.02.2015 Version: 22 Page: 8 / 10
Sort 24510 20515 21516 25510 2555 25412 2655 2766 21714 25510 +3S+0.02Mg N in relation to dry substance P 2 O 5 in relation to dry substance K 2 O soluble in water in relation to dry substance, Appearance total 24 20 21 25 25 25 26 27 21 25 ammonia 12.6 10.3 11.4 13 13 12.8 13.5 13.9 11.4 13.9 nitric 11.4 9.7 10.2 12 12 12.2 12.5 13.1 9.6 11.1 total 5 5 5 5 5 4 5 6 7 5 soluble in water 3 3 3 3 3 2.4 3 3.6 4.2 3 soluble in neutral ammonium citrate soluble in citric acid 2 from potassium chloride from potassium sulphate 4.5 4.5 4.5 4.5 4.5 3.6 4.5 5.4 6.3 4.5 4.9 4.9 4.9 4.9 4.9 3.9 4.9 5.8 6.9 4.9 10 15 16 10 5 12 5 6 Cl for the sorts with potassium sulphate, max 0.5 0.8 0.25 0.25 0.3 0.75 SO 3 soluble in water for the sorts with potassium sulphate, 8.5 12.8 13.6 8.5 5.1 11.9 9 Water content, max. 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 Granulometry between 1 4 mm, min. 95 95 95 95 95 95 95 95 95 95 below 1 and above 4 mm, max 5 5 5 5 5 5 5 5 5 5 Total combustible materials, max. 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 ph, min 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 S soluble in water 3 Mg, from dolomite, 0.02 MgO, 14 10 Date of issue: 23.02.2015 Version: 22 Page: 9 / 10
Sort 22612 +3S+0.2B+ 0.2Zn 161516 16168 18818 20717 141417 221010 16816 +2MgO 21712 N in relation to dry substance P 2 O 5 in relation to dry substance K 2 O soluble in water in relation to dry substance, Appearance total 22 16 16 18 20 14 22 16 21 ammonia 13.1 8.8 9 9.5 10.5 7.5 11.8 8.5 11 nitric 8.9 7.2 7 8.5 9.5 6.5 10.2 7.5 10 total 6 15 16 8 7 14 10 8 7 soluble in water 3.6 9 9.6 4.8 4.2 8.4 6 4.8 4.2 soluble in neutral ammonium citrate 5.4 13.5 14.4 7.2 6.3 12.6 9 7.2 6.3 soluble in citric acid 5.9 14.7 15.7 7.8 6.9 13.7 9.8 7.8 6.9 2 from potassium chloride from potassium sulphate 12 16 8 17 Cl for the sorts with potassium sulphate, max 0.8 0.85 0.5 0.6 SO 3 soluble in water for the sorts with potassium sulphate, 7.5 13.6 14.5 8.5 10.2 Water content, max. 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 between 1 4 mm, Granulometry min. 95 95 95 95 95 95 95 95 95 below 1 and above 4 mm, max 5 5 5 5 5 5 5 5 5 Total combustible materials, max. 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 ph, min 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 S soluble in water 3 B, from borax 0.2 Zinc, 0.2 MgO, 0.7 2 18 17 10 16 12 Date of issue: 23.02.2015 Version: 22 Page: 10 / 10