BS EN 16318-2013 Fertilizers Determination of trace elements Determination of chromiumVI by photometry method A and by ion chromatography with spectrophotometric detection method B.pdf

1、BSI Standards PublicationBS EN 16318:2013Fertilizers Determinationof trace elements Determination of chromium(VI)by photometry (method A) andby ion chromatography withspectrophotometric detection(method B)Copyright European Committee for Standardization Provided by IHS under license with CENNot for

2、ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 16318:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 16318:2013. It supersedes PD CEN/TS 16318:2012 which is withdrawn.The UK participation in its preparation was entrusted to

3、 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 necessary provisions of a contract. Users are responsible for its correct application.

4、 The British Standards Institution 2013. Published by BSI Standards Limited 2013ISBN 978 0 580 81662 8ICS 65.080Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 3

5、1 October 2013.Amendments/corrigenda issued since publicationDate Text affectedCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 16318:2013EUROPEAN STANDARD NORME EUROPENNE E

6、UROPISCHE NORM EN 16318 October 2013 ICS 65.080 Supersedes CEN/TS 16318:2012English Version Fertilizers - Determination of trace elements - Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B)Engrais - Dosage des lments traces

7、- Dosage du chrome (VI) par spectrophotomtrie (mthode A) et chromatographie ionique avec dtection spectrophotomtrique (mthode B) Dngemittel - Bestimmung von Elementspuren - Bestimmung von Chrom(VI) mit Photometrie (Verfahren A) und mit Ionenchromatographie mit spektrometrischer Detektion (Verfahren

8、B) This European Standard was approved by CEN on 15 September 2013. 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 bibliographica

9、l 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 responsibility o

10、f 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 Republic of Ma

11、cedonia, 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 NORMALISATION E

12、UROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16318:2013: ECopyright European Committee for Standardization Provided by IHS under

13、 license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 16318:2013EN 16318:2013 (E) 2 Contents Page 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Sampling and sample preparation .4 5 Method A: Determination by water extraction and s

14、pectrophotometric detection 5 5.1 Principle 5 5.2 Reagents .5 5.3 Apparatus .6 5.4 Procedure .6 5.4.1 Preparation of the test solution 6 5.4.2 Preparation of the blank test solution .7 5.4.3 Spectrophotometric measurement 7 5.5 Calculation and expression of the results 7 5.5.1 Calibration 7 5.5.2 Ca

15、lculation of the element content in the sample 7 6 Method B: Determination by alkaline digestion and ion chromatography with spectrophotometric detection 8 6.1 Principle 8 6.1.1 Digestion .8 6.1.2 Determination .8 6.1.3 Interferences and sources of error 9 6.2 Reagents .9 6.3 Apparatus 11 6.4 Alkali

16、ne digestion procedure 11 6.4.1 General . 11 6.4.2 Preparation of test solutions using a hotplate or heating block . 11 6.5 Procedure 12 6.5.1 Instrumental set-up. 12 6.5.2 Calibration . 12 6.5.3 Test solution measurement . 12 6.6 Quality control . 13 6.6.1 General . 13 6.6.2 Blank test solution 13

17、6.6.3 Verification of method 13 6.6.4 Duplicate samples 13 6.6.5 Cr(VI) spiked samples 13 6.6.6 Cr(III) spiked samples . 14 6.6.7 Interpretation of Quality Control data . 14 6.7 Calculation and expression of results 14 6.7.1 Calculation . 14 6.7.2 Expression of results . 15 7 Precision 15 8 Test rep

18、ort . 15 Annex A (informative) Results of the inter-laboratory test performed by VDLUFA on method A . 16 A.1 Inter-laboratory tests 16 A.2 Statistical results for the determination of chromium(VI) by photometry (method A) 16 Annex B (informative) Results of a validation study on spiked water samples

19、 17 Bibliography . 18 Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 16318:2013EN 16318:2013 (E) 3 Foreword This document (EN 16318:2013) has been prepared by Technical Co

20、mmittee 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 April 2014, and conflicting national standards shall

21、 be withdrawn at the latest by April 2014. 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 supersedes CEN/TS 16318:2012.

22、 This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. The following changes have been made to the former edition: the CEN Technical Specification has been adopted as a European Standard; a reference to Annex A has been added

23、 to Clause 7 concerning the results of inter-laboratory tests on the precision of method A; the statistical results of an inter-laboratory test performed by the Technical Group Fertilizers of the German VDLUFA have been added as Annex A (informative); the results of a validation study with spiked wa

24、ter samples have been added as Annex B (informative); the document has been editorially revised. 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, Cypr

25、us, Czech 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

26、 Kingdom. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 16318:2013EN 16318:2013 (E) 4 1 Scope This European Standard specifies two methods for the determination of the co

27、ntent of soluble chromate in fertilizers. 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 higher than 1 mg/kg. Method B specifies the determination of chromate by alkaline digestion and i

28、on chromatography with spectrophotometric detection. This method can be used to determine Cr(VI)-mass fractions in solids higher than 0,1 mg/kg. NOTE In case of reducing or oxidizing fertilizer matrix, no valid Cr(VI) content can be reported. 2 Normative references The following documents, in whole

29、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 liming materia

30、ls 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 15192:2006, Cha

31、racterisation 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 Terms and definitions For the purposes of this d

32、ocument, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 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 EN 1482-1 2. Sample preparation shall be carried out in accordan

33、ce 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. plastic, glass). After digestion, the sample shall be analyzed as soo

34、n as possible. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 16318:2013EN 16318:2013 (E) 5 5 Method A: Determination by water extraction and spectrophotometric detection

35、5.1 Principle Chromate is extracted from the sample with water at room temperature. The chromate concentration in the extract is measured by colorimetry using 1,5-diphenylcarbazide. When chromate reduces the 1,5-diphenylcarbazide a magenta coloured complex of 1,5-diphenylcarbazone and chromium is fo

36、rmed which can be measured colorimetrically at 540 nm. 5.2 Reagents Use only reagents of recognized analytical grade and water conforming to 5.2.1. 5.2.1 Water, according to EN ISO 3696, grade 2 (electrical conductivity max. 0,1 mS m-1equivalent to resistivity greater than 0,01 Mm at 25 C). It is re

37、commended that the water used is obtained from a purification system that delivers ultrapure water having a resistivity greater than 0,18 Mm. 5.2.2 Hydrochloric acid, c(HCl) = 12 mol/l; 37 % volume fraction, 1,18 g/ml. 5.2.3 Hydrochloric acid, diluted, c(HCl) approximately 6 mol/l. Mix equal volumes

38、 of hydrochloric acid (5.2.2) and water (5.2.1). 5.2.4 Diphenylcarbazide solution. Dissolve 1,0 g Diphenylcarbazide CO(NHNHC6H5)2 in 100 ml acetone and add one drop of acetic acid. If this solution is stored in a glass bottle in the dark at 4 C, it may be used for approximately two weeks. This solut

39、ion shall be clear without colour. If the diphenylcarbazide solution has become coloured, it shall be discarded and freshly prepared before use. 5.2.5 Chromate standard stock solution, (chromate) = 1 000 mg/l. Dissolve 2 829 mg potassium dichromate (K2Cr2O7) in 1 000 ml water (5.2.1) using a volumet

40、ric flask. This solution may be used for two weeks if stored in the dark at 4 C. 5.2.6 Chromate standard stock solution, (chromate) = 50 mg/l. Dilute 5 ml chromate stock solution (5.2.5) to 100 ml with water (5.2.1) using a volumetric flask. This solution shall be freshly prepared on the day of use.

41、 5.2.7 Standard solutions. Prepare the standard solutions by diluting aliquots of the 50 mg/l chromate standard stock solution (5.2.6) with water (5.2.1) in 100 ml volumetric flasks. The aliquots and final concentrations of chromate are given in Table 1. Other volumes and concentrations may be used

42、for the preparation of standard solutions if appropriate. See 5.4.3 for further instructions on how to prepare the standard solutions. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS

43、-,-,-BS EN 16318:2013EN 16318:2013 (E) 6 Table 1 Aliquots and final concentrations for the preparation of chromate standards from a 50 mg/l chromate standard stock solution in 100 ml volumetric flasks Aliquot Final concentration of chromate ml mg/l 0 0 (calibration blank) 0,05 0,025 0,20 0,10 0,50 0

44、,25 1,00 0,50 1,50 0,75 A blank solution shall be prepared in a separate volumetric flask by adding water (5.2.1) only. The standard solutions shall be prepared freshly on the day of use. 5.3 Apparatus 5.3.1 Common laboratory glassware. 5.3.2 Analytical balance, capable of weighing to an accuracy of

45、 1 mg. 5.3.3 Membrane filters and vacuum filtration apparatus. The filters should be made of cellulose nitrate, pore size 5 m and fit into the vacuum filtration apparatus. 5.3.4 Mechanical shaker. 5.3.5 Pipettes and/or dilutor, pipettes with fixed or variable volume and volumetric glassware to perfo

46、rm dilutions. Alternatively, a dilutor may be used, which is an instrument used for automated volumetric dilutions. The precision and accuracy of this equipment for volumetric dilutions shall be proved, controlled, and documented regularly. 5.3.6 Spectrophotometer, capable to measure transmitted lig

47、ht at 540 nm. 5.3.7 100 ml bottles, made from PE or PP, equipped with watertight caps. 5.4 Procedure 5.4.1 Preparation of the test solution Weigh approximately 10 g, to the nearest 0,01 g, of the prepared sample and transfer to a suitable extraction vessel (5.3.7). Add 40 ml of water (5.2.1). If the

48、 sample material (e.g. organic material) absorbs a high amount of water, add additionally water (5.2.1) to obtain a fluid suspension. Record the amount of additional water added. It may be necessary to use larger extraction vessels in such cases. Close the cap tightly and shake vigorously for 15 min

49、 on a mechanical shaker (5.3.4). Filter the suspension immediately through membrane filters with 5 m pore size using the vacuum filtration apparatus (5.3.3). Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-