Fertilizers - Determination of sulfates content using three different methods

This document specifies three different methods (Methods A, B and C) for the determination of sulfur present in fertilizers extracts in the form of sulfates. Method A specifies the gravimetric method. Method B specifies the method using inductively coupled plasma optical spectrometry (ICP-OES). Method C specifies the method using ion chromatography (IC).

Düngemittel - Bestimmung von Sulfat mit drei verschiedenen Verfahren

Diese Europäische Norm legt drei verschiedene Verfahren (Verfahren A, B und C) für die Bestimmung des in Düngemittelextrakten vorliegenden Schwefels in Form von Sulfaten fest. Als Verfahren A ist das gravimetrische Verfahren festgelegt. Als Verfahren B ist die Bestimmung mittels optischer Emissionsspektro¬metrie mit induktiv gekoppeltem Plasma (ICP OES) festgelegt. Als Verfahren C ist die Vorgehensweise mittels Ionenchromatographie (IC) festgelegt.

Engrais - Dosage des sulfates selon trois méthodes différentes

La présente norme européenne spécifie trois méthodes différentes (méthodes A, B et C) de dosage du soufre présent dans les extraits d’engrais sous forme de sulfate. La méthode A utilise la gravimétrie. La méthode B emploie la spectrométrie d’émission optique à plasma inductif (ICP-OES). La méthode C a recours à la chromatographie ionique (IC).

Gnojila - Določevanje sulfatov s tremi različnimi metodami

Ta evropski standard opredeljuje tri različne metode (Metodo A, B in C) za določanje žvepla, prisotnega v ekstraktih gnojil v obliki sulfatov. Metoda A določa gravimetrično metodo. Metoda B določa metodo z uporabo optične spektrometrije z induktivno sklopljeno plazmo (ICP-OES). Metoda C določa metodo z uporabo ionske kromatografije (IC).

General Information

Status
Withdrawn
Publication Date
27-Oct-2009
Withdrawal Date
09-Aug-2022
Current Stage
9960 - Withdrawal effective - Withdrawal
Completion Date
10-Aug-2022

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Sulfat mit drei verschiedenen VerfahrenEngrais - Dosage des sulfates selon trois méthodes différentesFertilizers - Determination of sulfates content using three different methods65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15749:2009SIST EN 15749:2010en,fr,de01-februar-2010SIST EN 15749:2010SLOVENSKI
STANDARDSIST-TS CEN/TS 15749:20081DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15749
October 2009 ICS 65.080 Supersedes CEN/TS 15749:2008English Version
Fertilizers - Determination of sulfates content using three different methods
Engrais - Dosage des sulfates selon trois méthodes différentes
Düngemittel - Bestimmung von Sulfat mit drei verschiedenen Verfahren This European Standard was approved by CEN on 20 September 2009.
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 bibliographical references concerning such national standards may be obtained on application to the CEN 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 of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15749:2009: ESIST EN 15749:2010

Statistical results of the inter-laboratory tests . 19Bibliography . 22 SIST EN 15749:2010

2 Normative references The following referenced documents are indispensable for the application of this document. 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 CEN/TS 15925, Fertilizers — Extraction of total sulfur present in various forms CEN/TS 15926, Fertilizers — Extraction of water soluble sulfur where the sulfur is in various forms CEN/TS 15960, Fertilizers — Extraction of total calcium, total magnesium, total sodium and total sulfur in the forms of sulfates CEN/TS 15961, Fertilizers — Extraction of water soluble calcium, magnesium, sodium and sulfur (in the forms of sulfates) EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) 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. 4 Principle 4.1 Method A: Gravimetric method Sulfur is extracted from the sample according to the methods described in CEN/TS 15925, CEN/TS 15926, CEN/TS 15960 or CEN/TS 15961 and determined based on the gravimetric determination as barium sulfate. 4.2 Method B: ICP-OES Sulfur is extracted from the sample according to the methods described in CEN/TS 15925, CEN/TS 15926, CEN/TS 15960 or CEN/TS 15961 and its concentration in the extract is measured by inductively coupled plasma-optical emission spectrometry (ICP-OES). SIST EN 15749:2010

Calculate the SO3 content, wSO3, as mass fraction in percent of the fertilizer according to Equation (2): 2,5SSO3×=ww (2) where m1 is the mass of the barium sulfate precipitate, in mg; m2 is the mass of the test portion, in g; v1 is the volume of the extraction solution, in ml; v2 is the aliquot volume, in ml. 7 Method B – ICP-OES method 7.1 Reagents Use only reagents of recognized analytical grade, and water conforming to grade 2 of EN ISO 3696. Stock solutions shall be replaced after a maximum of one year, but the standard solution shall be freshly prepared monthly as a minimum.
7.1.1 Hydrochloric acid, ρ approximately 1,18 g/ml; 7.1.2 Diluted hydrochloric acid, mix 40 ml of hydrochloric acid (7.1.1) in 1 l of water; 7.1.3 Sulfur stock solution, corresponding to 1 000 mg/l sulfur. Dry in a pre-treatment step some grams of sodium sulfate (Na2SO4) at 105 °C for 1 h. Let cool in a desiccator. Weigh to the nearest 0,1 mg, approximately 4,437 5 g of sodium sulfate (Na2SO4). Dissolve the weighted SIST EN 15749:2010

7.3 Preparation of the extract The sulfur is extracted from the sample according to one of the methods described in CEN/TS 15925, CEN/TS 15926, CEN/TS 15960 or CEN/TS 15961.
7.4 Procedure 7.4.1 General Calibration shall be performed by means of the standard addition technique. This method allows the analysis of fertilizers with unknown matrix composition or with a matrix that cannot be synthetically imitated easily. 7.4.2 Preparation of the test solution Dilute the extraction solution with the diluted hydrochloric acid (7.1.1) to obtain a concentration between 10 mg/l and 150 mg/l of sulfur. 7.4.3 Preparation of the blank test solution Carry out a blank test at the same time as the extraction, with only the reagents. 7.4.4 Preparation of the calibration solutions The additions to the test solution, prior to the dilution step, should be about 20 %, 50 % and 100 % of the expected sulfur content. After the additions, dilute each of the samples with the diluted hydrochloric acid (7.1.1). SIST EN 15749:2010
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