1、January 2013 Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS
2、 65.080!$gE“1936834www.din.deDDIN EN 16196Fertilizers Manganimetric determination of extracted calcium followingprecipitation in the form of oxalate;English version EN 16196:2012,English translation of DIN EN 16196:2013-01Dngemittel Manganometrische Bestimmung von Calcium nach Oxalatfllung;Englische
3、 Fassung EN 16196:2012,Englische bersetzung von DIN EN 16196:2013-01Engrais Dosage manganimtrique du calcium extrait aprs prcipitation sous forme doxalate;Version anglaise EN 16196:2012,Traduction anglaise de DIN EN 16196:2013-01SupersedesDIN CEN/TS 16196(DIN SPEC 91272):2011-08www.beuth.deIn case o
4、f doubt, the German-language original shall be considered authoritative.Document comprises 12 pages 12.12 DIN EN 16196:2013-01 2 A comma is used as the decimal marker. National foreword This document (EN 16196:2012) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming material
5、s” (Secretariat: DIN, Germany) under the mandate M/335. The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-03-02 AA Dngemittel. The method specifi
6、ed in this standard is based upon Regulation (EC) No 2003/2003 relating to fertilizers, Annex IV, method 8.6 (see Bibliography). The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DI
7、N CEN/TS 16196 (DIN SPEC 91272):2011-08 as follows: a) the status of the Technical Specification has been changed to that of a European Standard; b) the standard has been editorially revised. Previous editions DIN CEN/TS 16196 (DIN SPEC 91272): 2011-08 National Annex NA (informative) Bibliography DI
8、N ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16196 November 2012 ICS 65.080 Supersedes CEN/TS 16
9、196:2011English Version Fertilizers - Manganimetric determination of extracted calcium following precipitation in the form of oxalate Engrais - Dosage manganimtrique du calcium extrait aprs prcipitation sous forme doxalate Dngemittel - Manganometrische Bestimmung von Calcium nach Oxalatfllung This E
10、uropean Standard was approved by CEN on 6 October 2012. 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
11、 concerning such national standards may be obtained on application to the CEN-CENELEC 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 memb
12、er into its own language and notified to the CEN-CENELEC 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, Former Yugoslav Republic of Macedonia, Fra
13、nce, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES K
14、OMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16196:2012: EEN 16196:2012 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and defin
15、itions .44 Sampling .45 Principle 46 Reagents .47 Apparatus .58 Preparation of the test portion .59 Procedure .59.1 Preparation of the calcium oxalate 59.2 Titration of the oxalate precipitate .510 Calculation and expression of the result 511 Precision .611.1 Inter-laboratory test .611.2 Repeatabili
16、ty .611.3 Reproducibility .612 Test report 7Annex A (informative) Statistical results of the inter-laboratory tests 8Bibliography . 10DIN EN 16196:2013-01 EN 16196:2012 (E) 3 Foreword This document (EN 16196:2012) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”
17、, 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 May 2013, and conflicting national standards shall be withdrawn at the latest by May 2013. Attention is d
18、rawn 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 supersedes CEN/TS 16196:2011. The following changes have been made to the former editi
19、on: a) the CEN Technical Specification has been adopted as a European Standard; b) the document has been editorially revised. 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 Regulat
20、ions, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Ital
21、y, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16196:2013-01 EN 16196:2012 (E) 4 1 Scope This European Standard specifies a manganimetric method for the determination of th
22、e calcium content in fertilizer extracts. This method is applicable to EC fertilizers for which a declaration of the total and/or water-soluble calcium content is provided for in Regulation (EC) No 2003/2003, Annex I 3. 2 Normative references The following documents, in whole or in part, are normati
23、vely referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1482-2, Fertilizers and liming materials Sampling and sample
24、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 15960, Fertilizers Extraction of total
25、 calcium, total magnesium, total sodium and total sulfur in the forms of sulfates EN 15961, Fertilizers Extraction of water soluble calcium, magnesium, sodium and sulfur in the form of sulfates 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1:1
26、999 and EN 12944-2:1999 apply. 4 Sampling 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. Grinding of the laboratory sample is recommended for homogeneity reasons
27、. 5 Principle Precipitation of the calcium contained in an aliquot of the extraction solution in the form of an oxalate, which is determined by titration using potassium permanganate. 6 Reagents 6.1 Diluted hydrochloric acid, one volume of hydrochloric acid, = 1,18g/ml, and one volume of water. 6.2
28、Sulfuric acid, 1:10 diluted, one volume of sulfuric acid, = 1,84 g/ml, in ten volumes of water. 6.3 Ammonia solution, 1:1 diluted, one volume of ammonia, = 0,88 g/ml, and one volume of water. 6.4 Ammonia oxalate, (NH4)2 C2O4H2O, saturated solution at ambient temperature, approximately = 40 g/l. DIN
29、EN 16196:2013-01 EN 16196:2012 (E) 5 6.5 Citric acid solution, 30 % (mass concentration). 6.6 Ammonium chloride solution, 5 % (mass concentration). 6.7 Solution of bromothymol blue in ethanol, at 95 %, 0,1 % (mass concentration). 6.8 Solution of bromocresol green in ethanol, at 95 %, 0,04 % (mass co
30、ncentration). 6.9 Standard solution of potassium permanganate, c = 0,02 mol/l. 7 Apparatus 7.1 Filter crucible, with 5 m to 20 m porosity sintered glass. 7.2 Hot water bath. 7.3 400 ml beaker. 8 Preparation of the test portion Using a pipette, take an aliquot portion of the extraction solution obtai
31、ned according to EN 15960 or EN 15961, containing between 15 mg and 50 mg of Ca (= 21 mg to 70 mg of CaO). The volume of this aliquot is v2. Pour into a beaker (7.3). If necessary, neutralise, turning of indicator (6.7) from green to blue, with a few drops of the ammonia solution (6.3). Add 1 ml of
32、the citric acid solution (6.5) and 5 ml of ammonium chloride solution (6.6). 9 Procedure 9.1 Preparation of the calcium oxalate Add approximately 100 ml of water. Bring to the boil, add eight to ten drops of indicator solution (6.8) and, slowly, 50 ml of a hot ammonium oxalate solution (6.4). If a p
33、recipitate forms, dissolve by adding a few drops of hydrochloric acid (6.1). Neutralise very slowly with ammonia solution (6.3) while stirring continuously to a pH of 4,4 to 4,6, turning of indicator (6.8) from green to blue. Place the beaker in a boiling hot water bath (7.2) for approximately 30 mi
34、n. Remove the beaker from the bath, leave standing for 1 h and filter through the crucible (7.1). 9.2 Titration of the oxalate precipitate Wash the beaker and crucible until the excess ammonium oxalate has been completely removed (this can be checked by the absence of chloride in the washing water).
35、 Place the crucible in the beaker (7.3) and dissolve the precipitate with 50 ml of hot sulfuric acid (6.2). Add water to the beaker in order to obtain a volume of approximately 100 ml. Bring to a temperature of 70 C to 80 C and titrate drop by drop with a permanganate solution (6.9) until the pink c
36、olour lasts for a minute. This volume is v. 10 Calculation and expression of the result Calculate the calcium (Ca) content, wCa, in percent of the fertilizer analysed according to Formula (1). mvvtvw=21Ca0,0240,200 (1) where DIN EN 16196:2013-01 EN 16196:2012 (E) 6 v is the volume of permanganate us
37、ed, in millilitres; m is the mass of the test portion, in grams; v2is the aliquot volume, in millilitres; v1is the volume of the extraction solution, in millilitres; t is the substance concentration of the permanganate solution in moles per litre. CaO (%) = Ca (%) 1,400 11 Precision 11.1 Inter-labor
38、atory test Repeated inter-laboratory tests have been carried out in 2007 and 2009 with different numbers of participating laboratories and several different samples (see Table A.1 to Table A.4). Repeatability and reproducibility were calculated according to ISO 5725-2. The values derived from these
39、inter-laboratory tests may not be applicable to concentration ranges and matrices other than those given in Annex A. 11.2 Repeatability The absolute difference between two independent single test results, obtained with the same method on identical test material in the same laboratory by the same ope
40、rator using the same equipment within a short interval of time, will in not more than 5 % of the cases exceed the values of r given in Table 1 and Table 2. 11.3 Reproducibility The absolute difference between two single test results, obtained with the same method on identical test material in differ
41、ent laboratories by different operators using different equipment, will in not more than 5 % of the cases exceed values of R given in Table 1 and Table 2. DIN EN 16196:2013-01 EN 16196:2012 (E) 7 Table 1 Results ring test 2007 Sample Extraction methodx% r % R % CAN EN 15960 6,39 0,19 1,13 EN 15961 2
42、,49 0,38 1,85 NPK1:23-4-13+7SO3 EN 15960 0,51 0,08 0,43 EN 15961 0,36 0,07 0,31 NPK2:12-11-18+2+8 EN 15960 3,49 0,15 1,20 EN 15961 0,53 0,10 0,49 Table 2 Results ring test 2009 Sample Extraction methodx% r % R % CAN EN 15960 6,20 0,25 1,2 EN 15961 2,61 0,19 4,05 NPK:12-12-17S+2 EN 15960 5,80 0,13 0,
43、74 EN 15961 3,52 0,27 3,93 12 Test report The test report shall contain at least the following information: a) all information necessary for the complete identification of the sample; b) the test method used with reference to this document; c) the method of preparation of the extraction solution (EN
44、 15960 or EN 15961); d) the test results obtained; e) date of sampling and sampling procedure (if known); f) date when the analysis was finished; g) whether the requirement of the repeatability limit has been fulfilled; h) all operating details not specified in this document, or regarded as optional
45、, together with details of any incidents occurred when performing the method, which might have influenced the test result(s). DIN EN 16196:2013-01 EN 16196:2012 (E) 8 Annex A (informative) Statistical results of the inter-laboratory tests The precision of the method was established in 2007 and in 20
46、09 by Working Group 7 “Chemical analysis” of CEN/TC 260 “Fertilizers and liming materials” in several inter-laboratory tests evaluated in accordance with ISO 5725-2. The statistical results are given in Table A.1 to Table A.4. Table A.1 Statistical results of the inter-laboratory test in 2007 Extrac
47、tion method EN 15960 Parameter Sample CAN NPK1:23-4-13+7SO3 NPK2:12-11-18+2+8 Number of participating laboratories 14 11 13 Number of laboratories after elimination of outliers (accepted test results) 12 11 13 Mean value x (%) 6,39 0,51 3,49 Repeatability standard deviation sr(%) 0,07 0,03 0,06 RSDr
48、(%) 1,1 6,0 1,6Repeatability limit r (%) 0,19 0,08 0,15 Reproducibility standard deviation sR(%) 0,40 0,15 0,43 RSDR(%) 6,3 30,0 12,3 Reproducibility limit R (%) 1,13 0,43 1,20Table A.2 Statistical results of the inter-laboratory test in 2007 Extraction method EN 15961 Parameter Sample CAN NPK1:23-4-13+7SO3 NPK2:12-11-18+2+8 Number of participating laboratories 14 10 12 Number of laboratories after elimination of outliers (accepted test results) 14 10 1
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