DIN EN 16318-2016 Fertilizers and liming materials - Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B) G.pdf

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1、July 2016 English price group 12No 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 65.080!%XLB“2534131www.din.deDIN EN

2、 16318Fertilizers and liming materials Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B);English version EN 16318:2013+A1:2016,English translation of DIN EN 16318:2016-07Dngemittel und Kalkdnger Bestimmung von Chrom(VI) mit

3、Photometrie (Verfahren A) und mit Ionenchromatographie mit spektrometrischer Detektion (Verfahren B);Englische Fassung EN 16318:2013+A1:2016,Englische bersetzung von DIN EN 16318:2016-07Engrais et amendements minraux basiques Dosage du chrome (VI) par spectrophotomtrie (mthode A) et chromatographie

4、ionique avecdtection spectrophotomtrique (mthode B);Version anglaise EN 16318:2013+A1:2016,Traduction anglaise de DIN EN 16318:2016-07SupersedesDIN EN 16318:2014-02www.beuth.deDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.Document

5、 comprises 23 pages 06.16 2 A comma is used as the decimal marker. National foreword This document (EN 16318:2013+A1:2016) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials” (Secretariat: DIN, Germany) under the mandate M/418. The responsible German body involved

6、in its preparation was DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products), Working Committee NA 057-03-02 AA Dngemittel. Attention is brought to the fact that in Clause 4 “Sampling and sample preparation”, third paragraph, first

7、 sentence, the term “oxidation” (German term “Oxidation”) is to be replaced by “reduction” (German term “Reduktion”). The Working Committee was informed of this error by a German expert. The error was checked by the Chairman of the Committee and has been confirmed. The error was already in the previ

8、ous English version of EN 16318:2014 and was erroneously repeated in the German version. It is currently being determined by the responsible CEN Working Committee CEN/TC 260/WG 7 whether a Corrigendum needs to be issued. The DIN Standards corresponding to the International Standards referred to in t

9、his document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN EN 16318:2014-02 as follows: a) the title and scope have been extended to include liming materials; b) Clause 7 “Precision” has been extended to include liming materials. Previo

10、us editions DIN CEN/TS 16318 (DIN SPEC 10788): 2012-06 DIN EN 16318: 2014-02 DIN EN 16318:2016-073 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (tr

11、ueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN EN 16318:2016-074 This page is intentionally blank DIN EN 16318:2016-07EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16

12、318:2013+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

13、) par spectrophotomtrie (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 spektrometrischerDetektion (Verfahren B) This European Standard was approved

14、by CEN on 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 li

15、sts 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 language made by translation unde

16、r 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, Estonia, Finland, Former Y

17、ugoslav 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 EURO

18、PEN DE NORMALISATION 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

19、 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 Procedure. 7 5.4.1 Preparation of the

20、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 alkaline digestion and ion chromatogra

21、phy 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 using a hotplate or heating block

22、. 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 samples 15 6.6.6 Cr(III) spiked samples

23、 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 DIN EN 16318:2016-07EN 16318:2013+A1:2016 (E) 3 Annex A (informative) Results of the int

24、er-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 Bibliography . 19 DIN EN 16318:2016-07EN 1631

25、8:2013+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 a national standard, either by publication

26、 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 patent rights. CEN and/or CENELEC shall no

27、t 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 the text by tags !“. This document has been

28、 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 carcinogenic to humans.“ According to the CE

29、N/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 Macedonia, France, Germany, Greece, Hunga

30、ry, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16318:2016-07EN 16318:2013+A1:2016 (E) 5 1 Scope !This European Standard specifies two methods for

31、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 higher than 1 mg/kg. Method B specifies the dete

32、rmination 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, no valid Cr(VI) content can be reported. !NOT

33、E 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 are indispensable for its application. For dat

34、ed 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 preparation EN 12944-1:1999, Fertilizers and liming mate

35、rials 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, Cha

36、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

37、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 EN 1482-1 2. Sample preparation shall be carr

38、ied 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. plastic, glass). After digestion, the sample shall

39、 be analyzed as soon as possible. DIN EN 16318:2016-07EN 16318:2013+A1:2016 (E) 6 5 Method A: Determination by water extraction and spectrophotometric detection 5.1 Principle Chromate is extracted from the sample with water at room temperature. The chromate concentration in the extract is measured b

40、y colorimetry using 1,5-diphenylcarbazide. When chromate reduces the 1,5-diphenylcarbazide a magenta coloured complex of 1,5-diphenylcarbazone and chromium is formed which can be measured colorimetrically at 540 nm. 5.2 Reagents Use only reagents of recognized analytical grade and water conforming t

41、o 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 recommended that the water used is obtained from a purification system that delivers ultrapure water having a resistivity greater than 0,18 M

42、m. 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 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

43、 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 solution shall be clear without colour. If the diphenylcarbazide solution has become coloured, it shall be discarded and freshly prepared before

44、 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 volumetric 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

45、/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. 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

46、 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 for the preparation of standard solutions if appropriate. See 5.4.3 for further instructions on how to prepare the standard solutions. DIN

47、EN 16318:2016-07EN 16318:2013+A1:2016 (E) 7 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 0,5

48、0 0,25 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

49、 of 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 perform dilutions. Alternatively, a dilutor may be used, which is an instrument used for automated volumetric dilutions. The precision