EN 16318:2013+A1:2016

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel und Kalkdünger - Bestimmung von Chrom (VI) mit Photometrie (Verfahren A) und mit Ionenchromatographie mit spektrometrischer Detektion (Verfahren B)Engrais et amendements minéraux basiques - Dosage du chrome (VI) par spectrophotométrie (méthode A) et chromatographie ionique avec détection spectrophotométrique (méthode B)Fertilizers and liming materials - Determination of chromium(VI) by photometry (method A) and by ion chromatography with spectrophotometric detection (method B)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16318:2013+A1:2016SIST EN 16318:2013+A1:2016en,fr,de01-julij-2016SIST EN 16318:2013+A1:2016SLOVENSKI
STANDARDSIST EN 16318:20131DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16318:2013+A1
February
t r s x ICS
x wä r z r Supersedes EN
s x u s zã t r s uEnglish Version
Fertilizers and liming materials æ Determination of chromatography with spectrophotometric detection Engrais et amendements minéraux basiques æ Dosage t chromatographie ionique avec détection
Düngemittel und Kalkdünger æ Bestimmung von Chrom Ionenchromatographie mit spektrometrischer This European Standard was approved by CEN on
s w September
t r s u and includes Amendment
s approved by CEN on
s { December
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
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t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x u s zã t r s u ªA sã t r s x ESIST EN 16318:2013+A1:2016

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 Bibliography . 19
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 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 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 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 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 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. plastic, glass). After digestion, the sample shall be analyzed as soon as possible. SIST EN 16318:2013+A1:2016

³
sá s z 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 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 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/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 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. SIST EN 16318:2013+A1:2016

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 1 mg. 5.3.3 Membrane filters and vacuum filtration apparatus. The filters should be made of cellulose nitrate, pore size 5 µm 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 and accuracy of this equipment for volumetric dilutions shall be proved, controlled, and documented regularly. 5.3.6 Spectrophotometer, capable to measure transmitted light 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 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 SIST EN 16318:2013+A1:2016

Calculate the analyte concentration, cf, in the filtrate of the test portion using the slope b and the intersection a according to Formula (2): ffSacb−= (2) where Sf
is the net signal of the test solution.
5.5.2 Calculation of the element content in the sample Calculate the analyte concentration in the sample or the mass fraction of the analyte, wE, expressed in milligrams of analyte per kilogram of fertilizer according to Formula (3). SIST EN 16318:2013+A1:2016

6 Method B: Determination by alkaline digestion and ion chromatography with spectrophotometric detection 6.1 Principle 6.1.1 Digestion Cr(VI) is digested from the sample by an alkaline solution. To quantify the content of Cr(VI) in a solid matrix, the following three criteria shall be satisfied: a) the digestion solution shall solubilize all species of Cr(VI); b) the conditions of the digestion shall not induce reduction of native Cr(VI) to Cr(III); c) the method shall not cause oxidation of native Cr(III) contained in the sample to Cr(VI). The alkaline digestion described in this document meets these criteria for a wide spectrum of solid matrices. Under the alkaline conditions, neglect able reduction of Cr(VI) or oxidation of native Cr(III) is expected. The addition of Mg2+ in a phosphate buffer to the alkaline solution prevents air oxidation of trivalent chromium (see [7], [8] and [9]). NOTE Background on methods for the determination of Cr(VI) in solid samples is given in EN 15192:2006, Annex D and [10], [11], [8]. 6.1.2 Determination The quantification of Cr(VI) in the alkaline digestion solution should be performed using a suitable technique with appropriate accuracy. For this purpose, ion chromatography is used to separate Cr(VI) from interferences. Following this ion chromatographic separation, Cr(VI) is measured spectrophotometrically either at 365 nm (direct UV detection) or after post-column derivatization with 1,5-diphenylcarbazide in acid solution at 540 nm. Post-column deriva
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