BS EN 16199-2012 Fertilizers Determination of the sodium extracted by flame-emission spectrometry《肥料 火焰放射光谱式测定萃取纳含量》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16199:2012Fertilizers Determination of the sodium extracted by flame-emission spectrometryBS EN 16199:2012 BRITISH STANDARDNational forewordThis British Standard is the UK

2、implementation of EN 16199:2012. It supersedes DD CEN/TS 16199:2011, which is withdrawn.The UK participation in its preparation was entrusted to T e c h n i c a l C o m m i t t e e C I I / 3 7 , F e r t i l i s e r s a n d r e l a t e d c h e m i c a l s .A list of organizations represented on this

3、committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012. Published by BSI Standards Limited 2012.ISBN 978 0 580 78187 2 ICS

4、 65.080 Compliance with a British Standard cannot confer immunityfrom legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 December 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS EN 16199:2012EUROPEAN S

5、TANDARD NORME EUROPENNE EUROPISCHE NORM EN 16199 November 2012 ICS 65.080 Supersedes CEN/TS 16199:2011English Version Fertilizers - Determination of the sodium extracted by flame-emission spectrometry Engrais - Dosage du sodium extrait par spectromtrie dmission de flamme Dngemittel - Bestimmung von

6、extrahiertem Natrium mit Emissions-Flammenspektrometrie This European 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 a

7、ny alteration. Up-to-date lists and bibliographical references 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 langu

8、age made by translation under the responsibility of a CEN member 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

9、, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, 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 FO

10、R STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE 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 16199:2012: EBS EN 16199:2012EN 16199:2012 (E

11、) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 45 Sampling .46 Reagents .47 Apparatus .58 Preparation of the test solution 59 Procedure .610 Calculation and expression of the result 611 Precision .711.1 Inter-laboratory test .711.2 Repeatability .7

12、11.3 Reproducibility .712 Test report 7Annex A (informative) Statistical results of the inter-laboratory test 9Bibliography . 11BS EN 16199:2012EN 16199:2012 (E) 3 Foreword This document (EN 16199:2012) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secre

13、tariat 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 drawn to the

14、 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 16199:2011. The following changes have been made to the former edition: a) the

15、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 Regulations, the n

16、ational 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, Italy, Latvia,

17、Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16199:2012EN 16199:2012 (E) 4 1 Scope This European Standard specifies a method for the determination of the sodium content in fertilizer

18、 extracts by flame-emission spectrometry. The method is applicable to EC fertilizers for which a declaration of the sodium content is provided for in Regulation (EC) Nr 2003/2003, Annex I 3. 2 Normative references The following documents, in whole or in part, are normatively referenced in this docum

19、ent 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 preparation Part 2: Sample pr

20、eparation 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 calcium, total magnesium, to

21、tal 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 12944-1:1999 and EN 12944-2:1999 apply

22、. 4 Principle Following suitable dilution of the extract obtained according to EN 15960 or EN 15961, the sodium content of the solution is determined by flame-emission spectrometry. 5 Sampling Sampling is not part of the method specified in this document. A recommended sampling method is given in EN

23、 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. 6 Reagents 6.1 Diluted hydrochloric acid. Add one volume of hydrochloric acid for analysis (20= 1,18 g/ml) to one volume of water. 6.2 Aluminium ni

24、trate, Al(NO3)39H2O. 6.3 Caesium chloride, CsCl. 6.4 Anhydrous sodium chloride, NaCl. BS EN 16199:2012EN 16199:2012 (E) 5 6.5 Caesium chloride and aluminium nitrate solution. Dissolve in water 50 g of caesium chloride (6.3) and 250 g of aluminium nitrate (6.2) in a graduated flask (7.2). Make up to

25、volume with water and mix. 6.6 Standard sodium solution, (Na) = 1 mg/ml. Dissolve in water 2,542 g of sodium chloride (6.4) in a graduated flask (7.2). Add 10 ml of hydrochloric acid (6.1). Make up to volume with water and mix. 6.7 Calibration solutions. 6.7.1 Place 10 ml of standard solution (6.6)

26、in a graduated flask (7.3). Make up to volume and mix. Mass concentration of the solution, (Na) = 40 g/ml. 6.7.2 Place 0 ml, 5 ml, 10 ml, 15 ml, 20 ml, 25 ml of the intermediate solution (6.7.1) in graduated flasks (7.4). Add 10 ml of the solution (6.5). Make up to volume and mix. Mass concentration

27、 of the solutions, (Na) = 0 g/ml, 2 g/ml, 4 g/ml, 6 g/ml, 8 g/ml and 10 g/ml. 7 Apparatus 7.1 Spectrometer, equipped for flame emission, set at 589,3 nm. 7.2 1 000 ml graduated flask. 7.3 250 ml graduated flask. 7.4 100 ml graduated flasks. 8 Preparation of the test solution Depending upon the expec

28、ted sodium content of the extraction solution according to EN 15960 or EN 15961 (5 g of fertilizer in 500 ml), carry out the dilutions in accordance with Table 1. BS EN 16199:2012EN 16199:2012 (E) 6 Table 1 Preparation of the test solution Na2O % Na % Intermediate dilution Final dilution Degree of d

29、ilution Sample (ml) (v2) Dilution to ml (v3) Sample (ml) (v4) Dilution to ml 3 to 5 5 to 10 10 to 20 20 to 38 2,2 to 3,7 3,7 to 7,4 7,4 to 15 15 to 28 10 10 10 5 50 100 100 100 10 10 5 5 100 100 100 100 50 100 200 400 Make up the intermediate dilution with water. For the final dilution, add 10 ml of

30、 the solution (6.5) to the graduated flask (7.4). For a test portion of 1 g multiply the volume of the final dilution (v4) by 5. 9 Procedure Prepare the spectrometer (7.1) for the measurements at 589,3 nm. Calibrate the instrument by measuring the response of the calibration solutions (6.7.2). Then

31、adjust the sensitivity of the instrument to use its entire scale when the most concentrated calibration solution is used. Then measure the response of the test solution to be analysed (7.1). Repeat this operation three times. 10 Calculation and expression of the result Draw a calibration curve by pl

32、otting the average response for each calibration solution along the ordinate and the corresponding concentrations, expressed in micrograms per millilitre on the abscissa. Determine from this the sodium concentration of the test solution. Calculate the quantity of sodium from the standard solutions t

33、aking account of the levels of dilution. Express the results as a mass fraction in percent of the sample. Calculate the Na content as a mass fraction, wNa, in percent of the fertilizer according to Formula (1): mvvvvxw=24213Na10(1) Calculate the Na2O content as a mass fraction, wNa2O, in percent of

34、the fertilizer according to Formula (2): 1,348NaONa2= ww(2) where x is the mass concentration of the solution introduced into the spectrometer, in micrograms per millilitre; v1is the volume of the extraction solution in millilitres; v2is the aliquot volume in the intermediate dilution in millilitres

35、; v3is the volume of intermediate dilution in millilitres; v4is the aliquot volume, in millilitres, of the final dilution (to 100 ml); m is the mass of the test portion in grams. BS EN 16199:2012EN 16199:2012 (E) 7 11 Precision 11.1 Inter-laboratory test Repeated inter-laboratory tests have been car

36、ried 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 inter-laboratory tests may not be applicable to concentr

37、ation 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 operator using the same equipment within a short interval o

38、f time, will in not more than 5 % of the cases exceed the values of r given in Table 2 and Table 3. 11.3 Reproducibility The absolute difference between two single test results, obtained with the same method on identical test material in different laboratories by different operators using different

39、equipment, will in not more than 5 % of the cases exceed values of R given in Table 2 and Table 3. Table 2 Results ring test 2007 Sample Extraction methodx% r % R % KALI ROH EN 15960 30,2 0,9 4,4 EN 15961 29,8 0,44 1,4 NPK1:20+0+8+Na EN 15960 0,56 0,08 0,3 EN 15961 0,52 0,04 0,12 Table 3 Results rin

40、g test 2009 Sample Extraction methodx% r % R % NPK:12-12-17S+2 EN 15960 5,46 0,22 0,22 EN 15961 5,73 0,39 1,85 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 ref

41、erence to this document; c) the method of preparation of the extraction solution (EN 15960 or EN 15961); BS EN 16199:2012EN 16199:2012 (E) 8 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

42、repeatability limit has been fulfilled; h) all operating details not specified in this document, or regarded as optional, together with details of any incidents occurred when performing the method, which might have influenced the test result(s). BS EN 16199:2012EN 16199:2012 (E) 9 Annex A (informati

43、ve) Statistical results of the inter-laboratory test The precision of the method was established in 2007 and in 2009 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 resu

44、lts are given in Table A.1 and Table A.2. Table A.1 Statistical results of the inter-laboratory test in 2007 Parameter Sample KALI ROH NPK1:20+0+8+Na Extraction method EN 15960 EN 15961 EN 15960 EN 15961Number of participating laboratories 11 10 9 9 Number of laboratories after elimination of outlie

45、rs (accepted test results) 8 7 7 8 Mean value x (%) 30,2 29,8 0,56 0,52 Repeatability standard deviation sr(%) 0,3 0,16 0,03 0,01 RSDr(%) 1,0 0,5 5,0 3,0 Repeatability limit r (%) 0,9 0,44 0,08 0,04 Reproducibility standard deviation sR(%) 1,6 0,5 0,1 0,04 RSDR(%) 5,2 1,7 17,0 8,0 Reproducibility li

46、mit R (%) 4,4 1,4 0,3 0,12 BS EN 16199:2012EN 16199:2012 (E) 10 Table A.2 Statistical results of the inter-laboratory test in 2009 Parameter Sample NPK:12-12-17S+2 Extraction method EN 15960 EN 15961 Number of participating laboratories 5 5 Number of laboratories after elimination of outliers (accep

47、ted test results) 4 5 Mean value x (%) 5,46 5,73 Repeatability standard deviation sr(%) 0,08 0,14RSDr(%) 1,0 2,0 Repeatability limit r (%) 0,22 0,39Reproducibility standard deviation sR(%) 0,08 0,66 RSDR(%) 1,0 12,0Reproducibility limit R (%) 0,22 1,85 BS EN 16199:2012EN 16199:2012 (E) 11 Bibliograp

48、hy 1 EN 1482-1, Fertilizers and liming materials Sampling and sample preparation Part 1: Sampling 2 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 3 Regu

49、lation (EC) No 2003/2003 of the European Parliament and of the Council of 13 October 2003 relating to fertilisers, Official Journal L 304, 21/11/2003, p. 0001-0194, Annex I and Annex IV, method 8.10 This page deliberately left blankThis page deliberately left blankBSI is the independent national body responsible for preparing British Standards and other standards-related publications, information and services. It presents the UK view on standards in Europe and at the international lev