SIST EN 15909:2010

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Calcium und Formiat in Calcium-BlattdüngemittelnEngrais - Dosage du calcium et du formate dans les engrais calcium foliaireFertilizers - Determination of calcium and formate in calcium foliar fertilizers65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15909:2010SIST EN 15909:2010en,fr,de01-december-2010SIST EN 15909:2010SLOVENSKI
STANDARD



SIST EN 15909:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15909
June 2010 ICS 65.080 English Version
Fertilizers - Determination of calcium and formate in calcium foliar fertilizers
Engrais - Dosage du calcium et du formiate dans les engrais calcium pour pulvérisation foliaire
Düngemittel - Bestimmung von Calcium und Formiat in Calcium-Blattdüngemitteln This European Standard was approved by CEN on 29 April 2010.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15909:2010: ESIST EN 15909:2010



EN 15909:2010 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Terms and definitions .44Principle .44.1General .44.2Calcium .44.3Formate .54.4Chloride .55Reagents .56Apparatus .67Sampling and sample preparation .68Procedure .78.1Preparation of the test solution .78.2Determination of the calcium content (concentration C1) .78.3Determination of formate content (concentration C2) .88.3.1HPLC conditions .88.3.2Elution conditions.88.3.3Detection conditions .88.3.4Procedure .98.3.5Calculation .98.4Determination of chloride content (concentration C3) .98.4.1Instrument settings for the automatic titroprocessor (6.3) .98.4.2Stop conditions . 108.4.3Evaluation . 108.4.4Preparation of sodium chloride solution 0,01 mol/l (for blank value determination) . 108.4.5Preparation of methyl orange indicator solution . 108.4.6Procedure . 108.4.7Calculation . 118.4.8Adjustment of correction factor (titre) of 0,01 mol/l silver nitrate solution with sodium chloride (5.12) . 119Calculation and expression of the result . 129.1Stoichiometric data. 129.2Expression of the result . 129.3Determination of residual content of calcium (9.2.3) . 1210Precision . 1310.1Inter-laboratory test . 1310.2Repeatability . 1310.3Reproducibility . 1311Test report . 13Annex A (informative)
Statistical results of the inter-laboratory tests . 14Bibliography . 15 SIST EN 15909:2010



EN 15909:2010 (E) 3 Foreword This document (EN 15909:2010) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2010, and conflicting national standards shall be withdrawn at the latest by December 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 15909:2010



EN 15909:2010 (E) 4 1 Scope This European Standard specifies a method for the determination of the content of calcium and formate in calcium foliar fertilizers in the presence of calcium chloride. This is determined and calculated by individual analytical determination of the following components:  Calcium (Ca2+),  Chloride (Cl-),  Formate (HCOO-). The method is applicable to calcium foliar fertilizers with a calcium content of approximately 30 %. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 480-10, Admixtures for concrete, mortar and grout — Test methods — Part 10: Determination of water soluble chloride content EN 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 2: Terms relating to fertilizers
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Principle 4.1 General Three different analytical procedures are used for the determination of the components to be determined, calcium, formate and chloride, in calcium foliar fertilizers. The substances calcium formate and calcium chloride are calculated stoichiometrically from the analytical results determined in each case (4.2, 4.3 and 4.4) (see Clause 9). 4.2 Calcium The calcium content is determined complexometrically with the diluted sample in strongly alkaline solution by means of adjusted 0,1 mol/l EDTA solution (5.1) and the calcium-specific indicator, calconcarboxylic acid (8.2).
SIST EN 15909:2010



EN 15909:2010 (E) 5 4.3 Formate The formate content is determined isocratically by reversed phase HPLC on the basis of the diluted sample (see 8.3). Evaluation is carried out with external standard.
4.4 Chloride The chloride content is determined by potentiometric titration according to the following reaction (see 8.4); the sample is first diluted, acetone is added and then the sample is acidified with acetic acid: Cl- + Ag+: AgCl (solid) After each addition of AgNO3 the measured potentials are measured and recorded using a titroprocessor. The endpoint is reached when the differential quotient E/∆V, i. e. the potential change E observed for each volume step ∆V, reaches its greatest value. This point can be determined using a titroprocessor or voltmeter. In this titration the chloride ions which are determined include other water-soluble halogen ions apart from fluorides. The total halogen content is designated chloride content. See EN 480-10 for the principles. 5 Reagents Use only reagents of recognized analytical grade and distilled or demineralized water (grade 3 according to EN ISO 3696:1995). 5.1 EDTA solution, (ethylenedinitrilotetraacetic acid disodiumsalt dehydrate), c(EDTA) = 0,1mol/l.
5.2 Calcium carbonate, reference material for complexometry. 5.3 Calconcarboxylic acid, indicator for metal titration. 5.4 Methyl orange. 5.5 Sodium chloride, p. a. 5.6 Sodium hydroxide solution, p. a.,
= 45 %. 5.7 Water, purified. 5.8 Ortho-phosphoric acid, p. a., w = 85 %. 5.9 Formate standard solution, for ion chromatography,
= 1 000 mg/l1). 5.10 Silver nitrate solution, c(AgNO3) = 0,01 mol/l. 5.11 Diluted hydrochloric acid, p.a., dilute 1 volume of hydrochloric acid, w = 37 %, with 1 volume of water (5.7). 5.12 Sodium chloride, certified primary reference material. 5.13 Diluted acetic acid, dilute 1 volume of acetic acid, w = 98 % to 100 %, with 1 volume of water (5.7). 5.14 Acetone, p.a.
1) Fluka Art. No: 49897-100 ML-F is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. SIST EN 15909:2010



EN 15909:2010 (E) 6 5.15 Magnesium sulfate, anhydrous p.a. 6 Apparatus 6.1 Analytical balance, accuracy of ± 1 mg. 6.2 HPLC apparatus, equipped with an automatic sample injection system, UV detector and evaluation system. 6.3 Titroprocessor2). 6.3.1 Dosimat, 10 ml exchange unit, for 0,01 mol/l sodium chloride solution (8.4.4). 6.3.2 Dosimat, 20 ml exchange unit, for 0,01 mol/l silver nitrate solution (5.11). 6.3.3 Silver ring electrode3).
6.4 Volumetric flask, capacity 100 ml. 6.5 Volumetric flask, capacity 1 000 ml. 6.6 Bulb pipette, capacity 10 ml. 6.7 Bulb pipette, capacity 20 ml. 6.8 Bulb pipette, capacity 25 ml. 6.9 Bulb pipette, capacity 100 ml. 6.10 Burette, capacity 25 ml. 6.11 Agate mortar. 6.12 Magnetic stirrer. 6.13 Glass beaker, capacity 50 ml. 6.14 Glass beaker, capacity 250 ml. 6.15 Glass beaker, capacity 600 ml. 6.16 Weighing dishes. 7 Sampling and sample preparation Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2.
2) Metrohm DMS-Titrino 716 is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. 3) Metrohm 6.0430.100 is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. SIST EN 15909:2010



EN 15909:2010 (E) 7 8 Procedure 8.1 Preparation of the test solution Transfer approximately 1 000 mg ± 10 mg of the sample to be determin
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