EN 16318-2013 en Fertilizers and liming materials - Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B) (I.pdf

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1、BSI Standards PublicationFertilizers and liming materials Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B)BS EN 16318:2013+A1:2016BS EN 16318:2013+A1:2016 BRITISH STANDARDNational forewordThis British Standard is the UK imp

2、lementation of EN 16318:2013+A1:2016. It supersedes BS EN 16318:2013 which is withdrawn.The start and finish of text introduced or altered by amendment is indicated in the text by tags. Tags indicating changes to CEN text carry the number of the CEN amendment. For example, text altered by CEN amendm

3、ent A1 is indicated by .The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilisers and related chemicals.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necess

4、ary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 89467 1ICS 65.080Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was p

5、ublished under the authority of the Standards Policy and Strategy Committee on 31 October 2013.Amendments/corrigenda issued since publicationDate Text affected31 March 2016 Implementation of CEN amendment A1:2016. Standard title amendedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16318:2013+

6、A1 February 2016 ICS 65.080 Supersedes EN 16318:2013English Version Fertilizers and liming materials - Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B) Engrais et amendements minraux basiques - Dosage du chrome (VI) par spe

7、ctrophotomtrie (mthode A) et chromatographie ionique avec dtection spectrophotomtrique (mthode B) Dngemittel und Kalkdnger - Bestimmung von Chrom (VI) mit Photometrie (Verfahren A) und mit Ionenchromatographie mit spektrometrischer Detektion (Verfahren B) This European Standard was approved by CEN o

8、n 15 September 2013 and includes Amendment 1 approved by CEN on 19 December 2015. 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

9、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 language made by translation under the re

10、sponsibility 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, Estonia, Finland, Former Yugoslav

11、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 FOR STANDARDIZATION COMIT EUROPEN DE N

12、ORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16318:2013+A1:2016 EEN 16318:2013+A1:2016 (E) 2 Contents Page Europea

13、n foreword . 4 1 Scope 5 2 Normative references 5 3 Terms and definitions . 5 4 Sampling and sample preparation 5 5 Method A: Determination by water extraction and spectrophotometric detection . 6 5.1 Principle . 6 5.2 Reagents . 6 5.3 Apparatus . 7 5.4 Procedure. 7 5.4.1 Preparation of the test sol

14、ution . 7 5.4.2 Preparation of the blank test solution 8 5.4.3 Spectrophotometric measurement 8 5.5 Calculation and expression of the results 8 5.5.1 Calibration . 8 5.5.2 Calculation of the element content in the sample . 8 6 Method B: Determination by alkaline digestion and ion chromatography with

15、 spectrophotometric detection 9 6.1 Principle . 9 6.1.1 Digestion 9 6.1.2 Determination 9 6.1.3 Interferences and sources of error 10 6.2 Reagents 10 6.3 Apparatus 12 6.4 Alkaline digestion procedure 13 6.4.1 General . 13 6.4.2 Preparation of test solutions using a hotplate or heating block . 13 6.5

16、 Procedure 13 6.5.1 Instrumental set-up . 13 6.5.2 Calibration 13 6.5.3 Test solution measurement 14 6.6 Quality control 14 6.6.1 General . 14 6.6.2 Blank test solution . 14 6.6.3 Verification of method 14 6.6.4 Duplicate samples 14 6.6.5 Cr(VI) spiked samples 15 6.6.6 Cr(III) spiked samples 15 6.6.

17、7 Interpretation of Quality Control data . 15 6.7 Calculation and expression of results . 15 6.7.1 Calculation 15 6.7.2 Expression of results . 16 7 !Precision Inter-laboratory tests“ 16 8 Test report 16 BS EN 16318:2013+A1:2016EN 16318:2013+A1:2016 (E) 3 Annex A (informative) Results of the inter-l

18、aboratory test performed by VDLUFA on method A 17 A.1 Inter-laboratory tests 17 A.2 Statistical results for the determination of chromium(VI) by photometry (method A) . 17 Annex B (informative) Results of a validation study on spiked water samples 18 Bibliography . 19 BS EN 16318:2013+A1:2016EN 1631

19、8:2013+A1:2016 (E) 2 Contents Page European foreword . 4 1 Scope 5 2 Normative references 5 3 Terms and definitions . 5 4 Sampling and sample preparation 5 5 Method A: Determination by water extraction and spectrophotometric detection . 6 5.1 Principle . 6 5.2 Reagents . 6 5.3 Apparatus . 7 5.4 Proc

20、edure. 7 5.4.1 Preparation of the test solution . 7 5.4.2 Preparation of the blank test solution 8 5.4.3 Spectrophotometric measurement 8 5.5 Calculation and expression of the results 8 5.5.1 Calibration . 8 5.5.2 Calculation of the element content in the sample . 8 6 Method B: Determination by alka

21、line digestion and ion chromatography with spectrophotometric detection 9 6.1 Principle . 9 6.1.1 Digestion 9 6.1.2 Determination 9 6.1.3 Interferences and sources of error 10 6.2 Reagents 10 6.3 Apparatus 12 6.4 Alkaline digestion procedure 13 6.4.1 General . 13 6.4.2 Preparation of test solutions

22、using a hotplate or heating block . 13 6.5 Procedure 13 6.5.1 Instrumental set-up . 13 6.5.2 Calibration 13 6.5.3 Test solution measurement 14 6.6 Quality control 14 6.6.1 General . 14 6.6.2 Blank test solution . 14 6.6.3 Verification of method 14 6.6.4 Duplicate samples 14 6.6.5 Cr(VI) spiked sampl

23、es 15 6.6.6 Cr(III) spiked samples 15 6.6.7 Interpretation of Quality Control data . 15 6.7 Calculation and expression of results . 15 6.7.1 Calculation 15 6.7.2 Expression of results . 16 7 !Precision Inter-laboratory tests“ 16 8 Test report 16 BS EN 16318:2013+A1:2016EN 16318:2013+A1:2016 (E) 3 An

24、nex A (informative) Results of the inter-laboratory test performed by VDLUFA on method A 17 A.1 Inter-laboratory tests 17 A.2 Statistical results for the determination of chromium(VI) by photometry (method A) . 17 Annex B (informative) Results of a validation study on spiked water samples 18 Bibliog

25、raphy . 19 BS EN 16318:2013+A1:2016EN 16318:2013+A1:2016 (E) 4 European foreword This document (EN 16318:2013+A1:2016) 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

26、a national standard, either by publication of an identical text or by endorsement, at the latest by August 2016, and conflicting national standards shall be withdrawn at the latest by August 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of

27、patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document includes Amendment 1 approved by CEN on 2015-12-19. This document supersedes !EN 16318:2013“. The start and finish of text introduced or altered by amendment is indicated in t

28、he text by tags !“. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. !deleted text“ !WARNING Avoid any contact with the skin, ingestion or inhalation of Cr(VI) compounds. Cr(VI) compounds are genotoxic and potentially ca

29、rcinogenic to humans.“ 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, Former Yugoslav Republic of

30、 Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16318:2013+A1:2016EN 16318:2013+A1:2016 (E) 5 1 Scope !Thi

31、s European Standard specifies two methods for the determination of the content of soluble chromate in fertilizers and liming materials.“ Method A specifies the determination of chromate after extraction with water by photometry. This method can be used to determine Cr(VI)-mass fractions in solids hi

32、gher than 1 mg/kg. Method B specifies the determination of chromate by alkaline digestion and ion chromatography with spectrophotometric detection. This method can be used to determine Cr(VI)-mass fractions in solids higher than 0,1 mg/kg. !NOTE 1“ In case of reducing or oxidizing fertilizer matrix,

33、 no valid Cr(VI) content can be reported. !NOTE 2 The term fertilizer is used throughout the body of this European Standard and includes liming materials unless otherwise indicated.“ 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and

34、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 preparatio

35、n 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 12944-3:2001, Fertilizers and liming materials Vocabulary Part 3: Terms re

36、lating to liming materials“ EN 15192:2006, Characterisation of waste and soil Determination of Chromium(VI) in solid material by alkaline digestion and ion chromatography with spectrophotometric detection EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Te

37、rms and definitions !For the purposes of this document, the terms and definitions given in EN 12944-1:1999, EN 12944-2:1999 and EN 12944-3:2001 apply.“ 4 Sampling and sample preparation Sampling is not part of the methods specified in this European Standard. A recommended sampling method is given in

38、 EN 1482-1 2. Sample preparation shall be carried out in accordance with EN 1482-2. Reasonable precautions have to be taken to prevent oxidation of chromate present in the sample. Samples shall be taken using appropriate devices and placed in containers that do not contain stainless steel (e.g. plas

39、tic, glass). After digestion, the sample shall be analyzed as soon as possible. BS EN 16318:2013+A1:2016EN 16318:2013+A1:2016 (E) 4 European foreword This document (EN 16318:2013+A1:2016) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which

40、 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 August 2016, and conflicting national standards shall be withdrawn at the latest by August 2016. Attention is drawn to the possibil

41、ity 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 includes Amendment 1 approved by CEN on 2015-12-19. This document supersedes !EN 16318:2013“. The start an

42、d finish of text introduced or altered by amendment is indicated in the text by tags !“. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. !deleted text“ !WARNING Avoid any contact with the skin, ingestion or inhalation o

43、f Cr(VI) compounds. Cr(VI) compounds are genotoxic and potentially carcinogenic to humans.“ 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, C

44、zech Republic, Denmark, 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 the United King

45、dom. BS EN 16318:2013+A1:2016EN 16318:2013+A1:2016 (E) 5 1 Scope !This European Standard specifies two methods for the determination of the content of soluble chromate in fertilizers and liming materials.“ Method A specifies the determination of chromate after extraction with water by photometry. Th

46、is method can be used to determine Cr(VI)-mass fractions in solids higher than 1 mg/kg. Method B specifies the determination of chromate by alkaline digestion and ion chromatography with spectrophotometric detection. This method can be used to determine Cr(VI)-mass fractions in solids higher than 0,

47、1 mg/kg. !NOTE 1“ In case of reducing or oxidizing fertilizer matrix, no valid Cr(VI) content can be reported. !NOTE 2 The term fertilizer is used throughout the body of this European Standard and includes liming materials unless otherwise indicated.“ 2 Normative references The following documents,

48、in whole or in part, are normatively 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 limin

49、g 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 12944-3:2001, Fertilizers and liming materials Vocabulary Part 3: Terms relating to liming materials“ EN 15192:2006, Characterisation of waste and soil Determination of Chromium(VI) in solid material by alkaline digestion and ion chro