EN 15909-2010 en Fertilizers - Determination of calcium and formate in calcium foliar fertilizers《肥料 钙和钙叶面肥甲酸的测定》.pdf

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1、BS EN 15909:2010ICS 65.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDFertilizers Determination ofcalcium and formatein calcium foliarfertilizersThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 June2010

2、 BSI 2010ISBN 978 0 580 65809 9Amendments/corrigenda issued since publicationDate CommentsBS EN 15909:2010National forewordThis British Standard is the UK implementation of EN 15909:2010.The UK participation in its preparation was entrusted to TechnicalCommittee CII/37, Fertilisers and related chemi

3、cals.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfro

4、m legal obligations.BS EN 15909:2010EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE 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 pulvrisation f

5、oliaire Dngemittel - Bestimmung von Calcium und Formiat in Calcium-Blattdngemitteln 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

6、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

7、 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 Republ

8、ic, 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. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE N

9、ORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, 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: EBS EN 15909:2010EN 15909:2010 (E) 2 Contents Page Foreword 31 Scope

10、42 Normative references 43 Terms and definitions .44 Principle 44.1 General 44.2 Calcium .44.3 Formate .54.4 Chloride 55 Reagents .56 Apparatus .67 Sampling and sample preparation .68 Procedure .78.1 Preparation of the test solution 78.2 Determination of the calcium content (concentration C1) 78.3 D

11、etermination of formate content (concentration C2) .88.3.1 HPLC conditions 88.3.2 Elution conditions88.3.3 Detection conditions .88.3.4 Procedure .98.3.5 Calculation 98.4 Determination of chloride content (concentration C3) 98.4.1 Instrument settings for the automatic titroprocessor (6.3) .98.4.2 St

12、op conditions . 108.4.3 Evaluation 108.4.4 Preparation of sodium chloride solution 0,01 mol/l (for blank value determination) 108.4.5 Preparation of methyl orange indicator solution 108.4.6 Procedure 108.4.7 Calculation . 118.4.8 Adjustment of correction factor (titre) of 0,01 mol/l silver nitrate s

13、olution with sodium chloride (5.12) 119 Calculation and expression of the result . 129.1 Stoichiometric data. 129.2 Expression of the result . 129.3 Determination of residual content of calcium (9.2.3) 1210 Precision 1310.1 Inter-laboratory test 1310.2 Repeatability 1310.3 Reproducibility 1311 Test

14、report . 13Annex A (informative) Statistical results of the inter-laboratory tests . 14Bibliography . 15BS EN 15909:2010EN 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

15、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 t

16、hat 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 Associati

17、on 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, Irel

18、and, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15909:2010EN 15909:2010 (E) 4 1 Scope This European Standard specifies a method for the determination of the content of calci

19、um 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 calci

20、um 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) a

21、pplies. 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 improve

22、rs 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 t

23、his 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 ca

24、lcium 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

25、mol/l EDTA solution (5.1) and the calcium-specific indicator, calconcarboxylic acid (8.2). BS EN 15909:2010EN 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 stan

26、dard. 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 AgNO3the measured potentials

27、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 ion

28、s 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

29、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

30、 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 %,

31、 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 comm

32、ercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. BS EN 15909:2010EN 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, equipp

33、ed 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)

34、. 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 Glas

35、s 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 ca

36、rried 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

37、 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. BS EN 15909:2010EN 15909:2010 (E) 7 8 Procedure 8.1 Preparation of the test solution Transfer approximately 1 000 mg 10 m

38、g of the sample to be determined, accurately weighed to 0,1 mg, to a weighing dish (6.16) (weight m). Transfer the test portion from the weighing dish to the volumetric flask (6.5) by rinsing with distilled water. Make the volumetric flask up to the mark with distilled water at 20C, and dissolve (so

39、lution R1). 8.2 Determination of the calcium content (concentration C1) 8.2.1 Using a bulb pipette (6.9), transfer 100 ml of solution R1 (8.1) to a glass beaker (6.15), and make up to 400 ml with distilled water. 8.2.2 Render the solution alkaline (pH 12) with 10 ml of sodium hydroxide solution (5.6

40、). 8.2.3 Add approximately 0,3 g of indicator (8.2.6) to the alkaline solution and, immediately after dissolution, titrate with adjusted EDTA solution (5.1) until the colour changes from red to green (6.10 and 6.12). Consumption: ml 0,1 mol/l EDTA solution (V1). The colour change can be improved sig

41、nificantly by adding a spatula tipful (approximately 20 mg to 40 mg) of magnesium sulfate (5.15). 8.2.4 Blank value: proceed as described in 8.2.2 and 8.2.3 with 400 ml of distilled water. Consumption: ml 0,1 mol/l EDTA solution (V2). 8.2.5 Calculation Calculate the calcium content, wCa, in percent

42、(mass fraction) according to the following equation: mtVVw=000 110010008 4,)(Ca21(1) where V1is the consumption of 0,1 mol/l EDTA solution for sample, in millilitre; V2is the consumption of 0,1 mol/l EDTA solution for blank value, in millilitre; 4,008 is 1/10 g/mol calcium; t is the correction facto

43、r for 0,1 mol/l EDTA solution; 10 is the aliquot portion; 100 is the factor for conversion to percent; 1 000 is the 0,1 mol/l EDTA solution (stoichiometric to 1/10 g/mol calcium) in millilitre; m is the mass of the test portion in grams (8.1). 8.2.6 Preparation of the indicator Triturate 0,10 g of c

44、alconcarboxylic acid (5.3), 0,05 g of methyl orange (5.4) and 9,85 g of sodium chloride (5.5) in the agate mortar (6.11) to a homogenous powder. 8.2.7 Adjustment of correction factor (titre), for 0,1 mol/l EDTA solution (5.1) BS EN 15909:2010EN 15909:2010 (E) 8 Transfer 0,19 g to 0,21 g of calcium c

45、arbonate (5.2), accurately weighed to 0,1 mg, to a glass beaker (6.15), and dissolve in 50 ml of distilled water, if necessary adding a few drops of hydrochloric acid (5.11) until the solution is clear. Dry the calcium carbonate (5.2) at 120C for at least 2 h before use. Subsequently, make up to 400

46、 ml with distilled water, and proceed as described in 8.2.2 to 8.2.4. Calculate the correction factor, t, according to the following equation: 10,009)(000 1211=VVmt (2) where t is the correction factor (titre) of 0,1 mol/l EDTA solution; 1 000 is the 0,1 mol/l EDTA solution (stoichiometric to 1/10 g

47、/mol calcium carbonate), in millilitre; V1is the consumption of 0,1 mol/l EDTA solution for calcium carbonate, in millititre; V2is the consumption of 0,1 mol/l EDTA solution for blank value, in millilitre; 10,009 is 1/10 g/mol calcium carbonate; m1is the weight of calcium carbonate (5.2), in grams.

48、8.3 Determination of formate content (concentration C2) 8.3.1 HPLC conditions Separation column4), particle size 5 m, 250 mm 4 mm, Eluent: phosphoric acid 0,5 % (8.3.4.1). 8.3.2 Elution conditions Flow rate: 1,5 ml/min; Column temperature: 30 C; Elution type: isocratic Injection volume: 20 l; Run ti

49、me: 5 min; Retention time of component to be determined: approximately 2 min; 8.3.3 Detection conditions Type: UV; Measurement wavelength: 214 nm. 4) LiChrospher 100 RP-8 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 th