EN 15705:2010
(Main)Fertilizers - Determination of urea condensates using high-performance liquid chromatography (HPLC) - Isobutylidenediurea and crotonylidenediurea (method A) and methylen-urea oligomers (method B)
Fertilizers - Determination of urea condensates using high-performance liquid chromatography (HPLC) - Isobutylidenediurea and crotonylidenediurea (method A) and methylen-urea oligomers (method B)
Fertilizers containing the condensates of urea and specified aldehydes (with crotonaldehyde called crotonyliden diurea or CDU, with isobutyraldehyde called isobutylidene diurea or IBDU, with formaldehyde called urea formaldehyde or methylene urea or MU) are covered by Annex I of the Regulation (EC) 2003/2003 [1] as nitrogenous fertilizers. The methods described in this European Standard enable the quantitative determination of these condensates and the determination of the solubility of the MU-oligomers according to the Regulation.
Düngemittel - Bestimmung von Harnstoffkondensaten mit Hochleistungs-Flüssigchromatographie (HPLC) - Isobutylidendiharnstoff und Crotonylidendiharnstoff (Verfahren A) und Methylenharnstoff-Oligomere (Verfahren B)
Diese Europäische Norm legt Verfahren für die Bestimmung von Isobutylidendiharnstoff (IBDU), Crotony-lidendiharnstoff (CDU) (Verfahren A) und Methylenharnstoff-Oligomere (MU) (Verfahren B) in Düngemitteln mit Hochleistungs-Flüssigchromatographie (HPLC) fest.
Das Verfahren gilt für alle Düngemittel, die keine störenden organischen Verbindungen enthalten.
Engrais - Dosage des condensats d'urée par chromatographie liquide haute performance (HPLC) - Isobutylidène diurée et crotonylidène diurée (méthode A) et oligomères de méthylène-urée (méthode B)
La présente Norme européenne spécifie les méthodes de dosage de l’isobutylidène diurée (IBDU), de la
crotonylidène diurée (CDU) (méthode A) et des oligomères de méthylène-urée (MU) (méthode B) dans les
engrais par chromatographie liquide haute performance (HPLC).
La méthode est applicable à tous les engrais qui ne contiennent pas de composés organiques interférents.
Gnojila - Določevanje kondenzatov sečnine s tekočinsko kromatografijo visoke ločljivosti (HPLC) - Izobutilidendiurea in krotonilidendiurea (metoda A) in oligomeri metilenuree (metoda B)
Ta evropski standard določa metode za določevanje izobutilidendiura(IBDU), krotonilidendiurea(CDU) (metoda A) ter oligomeri metilenuree (MU) (metoda B) v gnojilih s tekočinsko kromatografijo visoke ločljivosti (HPLC). Metoda se uporablja za vsa gnojila, ki ne vsebujejo motečih organskih spojin.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Harnstoffkondensaten mit Hochleistungs-Flüssigchromatographie (HPLC) - Isobutylidendiharnstoff und Crotonylidendiharnstoff (Verfahren A) und Methylenharnstoff-Oligomere (Verfahren B)Engrais - Dosage des condensats d'urée par chromatographie liquide haute performance (HPLC) - Isobutylidène diurée et crotonylidène diurée (méthode A) et oligomères de méthylene-urée (méthode B)Fertilizers - Determination of urea condensates using high-performance liquid chromatography (HPLC) - Isobutylidenediurea and crotonylidenediurea (method A) and methylene-urea oligomers (method B)65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15705:2010SIST EN 15705:2010en,fr,de01-oktober-2010SIST EN 15705:2010SLOVENSKI
STANDARDSIST-TS CEN/TS 15705:20091DGRPHãþD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15705
March 2010 ICS 65.080 Supersedes CEN/TS 15705:2009English Version
Fertilizers - Determination of urea condensates using high-performance liquid chromatography (HPLC) - Isobutylidenediurea and crotonylidenediurea (method A) and methylen-urea oligomers (method B)
Engrais - Dosage des condensats d'urée par chromatographie liquide haute performance (HPLC) - Isobutylidène diurée et crotonylidène diurée (méthode A) et oligomères de méthylène-urée (méthode B)
Düngemittel - Bestimmung von Harnstoffkondensaten mit Hochleistungs-Flüssigchromatographie (HPLC) - Isobutylidendiharnstoff und Crotonylidendiharnstoff (Verfahren A) und Methylenharnstoff-Oligomere (Verfahren B) This European Standard was approved by CEN on 21 February 2010.
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, Croatia, 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.
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B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15705:2010: ESIST EN 15705:2010
Results of the inter-laboratory tests . 15Annex B (informative)
Chromatogram and calibration curves method A . 17Annex C (informative)
Chromatogram and calibration curves method B . 19Bibliography . 22 SIST EN 15705:2010
1 Scope This European Standard specifies methods for the determination of isobutylidenediurea (IBDU), crotonylidenediurea (CDU) (method A) and methylene-urea oligomers (MU) (method B) in fertilizers using high-performance liquid chromatography (HPLC). The method is applicable to all fertilizers which do not contain interfering organic compounds. 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 EN ISO 3696:1995, 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 Sampling and sample preparation Sampling is not part of the method specified in this European Standard. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. 5 Method A: Determination of CDU and IBDU 5.1 Principle The sample is extracted with water and, after appropriate dilution, analyzed using a suitable HPLC system. 5.2 Reagents 5.2.1 Reagents of recognized analytical grade and distilled or demineralized water (grade 3 according to EN ISO 3696:1995). 5.2.2 Acetonitrile, p.a., HPLC-grade. SIST EN 15705:2010
1) LiChrosorb RP-18 7 µm 250/4 mm is an example of a suitable product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN or CENELEC of this product. SIST EN 15705:2010
5.4.3 Preparation of the test portion Weigh 1 g of the sample grounded to < 0,2 mm to the nearest 0,1 mg and flush into a 1 000 ml volumetric flask with water (5.2.1). Fill the flask to an amount of approximately 900 ml and treat it for 10 min in the ultrasonic bath (5.3.4). Then make up to the mark and stir for 1 h at room temperature on a magnetic stirrer (5.3.5). Dilute 10 ml of the solution in a 100 ml volumetric flask and filter into the HPLC injection vial through a disposable filter (5.3.6). 5.4.4 Measurement Measurement is performed manually or by means of an automatic sample loading system (autosampler). 5.4.5 Important annotations IBDU is able to form urea in aqueous solution. Therefore, the measurement of the calibration and sample solutions shall be completed within one working day. The concentrations of CDU and IBDU in the sample solutions shall be kept within the calibration limits (5.4.2) to ensure sufficient reproducibility. 5.5 Calculation The calculation can be performed manually or by means of a PC using the calibration parameters in respect to the amount used. In the case of PC-aided (computerized) calculation and application of Table 1 regarding the amounts of stock solution, the content of IBDU/CDU in milligrams per litre will be calculated by the system. The calculated values are equal to the percentage mass concentration of IBDU/CDU in the analysed sample of fertilizer. Following general rules for declaration in regulations to declare the content of the compounds as percentage mass fraction of nitrogen, calculate the contents, wN(IBDU)/wN(CDU) in percent (g/100 g), according to the following equations: 322,0IBDU(IBDU)N×=ww (1) SIST EN 15705:2010
2) The standard substance
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