SIST EN 16847:2016
(Main)Fertilizers - Determination of complexing agents in fertilizers - Identification of heptagluconic acid by chromatography
Fertilizers - Determination of complexing agents in fertilizers - Identification of heptagluconic acid by chromatography
This European Standard specifies a chromatographic method which allows the identification of heptagluconic acid (HGA) in fertilizers containing heptagluconic acid metal complexes.
This method is applicable to EC fertilizers containing complexed micro-nutrients, which are covered by Regulation (EC) No 2003/2003 [1].
Düngemittel - Bestimmung von Komplexbildnern in Düngemitteln - Bestimmung von Heptaglukonsäure mit Chromatographie
Diese Europäische Norm legt ein chromatographisches Verfahren zur Identifizierung von Heptaglukonsäure (HGA) in Düngemitteln fest, die Heptaglukonsäure-Metallkomplexe enthalten.
Dieses Verfahren gilt für Düngemittel mit komplexgebundenen Spurennährstoffen die den Anforderungen der Verordnung (EG) Nr. 2003/2003 [1] unterliegen.
Engrais - Détermination des agents complexants dans les engrais - Identification de l'acide heptagluconique par chromatographie
La présente norme européenne spécifie une méthode d'identification par chromatographie de l'acide heptagluconique (HGA) dans les engrais contenant des complexes métalliques de l’acide heptagluconique.
Cette méthode s'applique aux engrais CE contenant des oligoéléments complexés qui sont couverts par le Règlement (CE) n° 2003/2003 [1].
Gnojila - Določevanje kompleksirajočih agensov v gnojilih - Prepoznavanje heptaglukonske kisline s kromatografijo
Ta evropski standard določa kromatografsko metodo, ki omogoča prepoznavanje heptaglukonske kisline (HGA) v gnojilih, ki vsebujejo kovinske komplekse heptaglukonske kisline.
Ta metoda se uporablja za gnojila ES, ki vsebujejo kompleksna mikrohranila, obravnavana v Uredbi (ES) št. 2003/2003 [1].
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.]QDYDQMHDüngemittel - Bestimmung von Komplexbildnern in Düngemitteln - Bestimmung von Heptaglukonsäure mit ChromatographieEngrais - Détermination des agents complexants dans les engrais - Identification de l'acide heptagluconique par chromatographieFertilizers - Determination of complexing agents in fertilizers - Identification of heptagluconic acid by chromatography65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16847:2016SIST EN 16847:2016en,fr,de01-december-2016SIST EN 16847:2016SLOVENSKI
STANDARD
SIST EN 16847:2016
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16847
January
t r s x ICS
x wä r z r English Version
Fertilizers æ Determination of complexing agents in fertilizers æ Identification of heptagluconic acid by chromatography Engrais æ Détermination des agents complexants dans les engrais æ Identification de l 5acide heptagluconique par chromatographie
Düngemittel æ Bestimmung von Komplexbildnern in Düngemitteln æ Identifikation von Heptaglukonsäure mit Chromatographie This European Standard was approved by CEN on
s y November
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
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
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CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
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 z v yã t r s x ESIST EN 16847:2016
EN 16847:2016 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Terms and definitions . 4 4 Principle . 4 5 Interferences . 4 6 Apparatus . 5 7 Reagents . 5 7.1 Water, . 6 7.2 Sample preparation solvent. . 6 7.3 HGA stock solution, . 6 7.4 Eluent A: ortho-phosphoric acid, . 6 7.5 Eluent B: acetonitrile (HPLC-grade). . 6 8 Procedure. 6 8.1 Preparation of the HGA-metal complex sample solution . 6 8.2 Preparation of the calibration solutions . 7 8.3 Chromatographic analysis . 7 9 Calculation of the heptagluconic acid content and expression of the results . 8 10 Precision . 8 10.1 Inter-laboratory test . 8 10.2 Repeatability . 8 10.3 Reproducibility . 8 11 Test report . 9 Annex A (informative)
Chromatograms of the standard and a typical sample solution . 10 Annex B (informative)
Absorption spectra of the HGA . 12 Annex C (informative)
Calculation of the molar ratio HGA:Metal . 13 Annex D (informative)
Statistical results of the inter-laboratory test . 14 D.1 Inter-laboratory test . 14 D.2 Test Samples . 14 D.3 Inter-laboratory test procedure . 14 D.4 Results and statistical interpretation . 14 Annex E (informative)
Complete names of chelating agents . 16 Bibliography . 17
SIST EN 16847:2016
EN 16847:2016 (E) 3 European foreword This document (EN 16847:2016) 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 of an identical text or by endorsement, at the latest by July 2016, and conflicting national standards shall be withdrawn at the latest by July 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 not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. 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, Cyprus, 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 Kingdom. SIST EN 16847:2016
EN 16847:2016 (E) 4 1 Scope This European Standard specifies a chromatographic method which allows the identification of heptagluconic acid (HGA) in fertilizers containing heptagluconic acid metal complexes. This method is applicable to EC fertilizers containing complexed micro-nutrients, which are covered by Regulation (EC) No 2003/2003 [1]. NOTE For the complete names of the chelating agents mentioned in this document, see Annex E. 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 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, 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 and EN 12944-2:1999 apply. 4 Principle The method is based on demetalation with phosphoric acid of the micronutrient HGA complex present in an aqueous solution of the sample. The complexing agent is then identified and determined by high-performance liquid chromatography. The separation is carried out on an NH2 phase bonded to silica column and an aqueous solution of phosphoric acid and acetonitrile as eluent. The detection is based on UV photometry at 210 nm. 5 Interferences a) High concentrations of phosphate in the sample solution can create a large peak preventing the identification/determination of HGA. b) High concentrations of chloride, sulfate and nitrate do not interfere in the identification/determination of the complexing agent. c) The presence of the chelates of EDDHSA, [o,o]EDDHA, [o,o]EDDHMA, EDTA, DTPA, CDTA, HEEDTA, IDHA as well as the corresponding chelating agents do not interfere since they are separated from HGA.
These substances can be detected in the chromatogram by the appearance of a peak at larger retention times. Therefore, the presence of these kinds of substances shall be taken into account when successive injections are scheduled. SIST EN 16847:2016
EN 16847:2016 (E) 5 d) The presence of gluconic acid does interfere in the determination of the complexing agent. e) The presence of aspartic acid, humic substances and lignosulfonic acid may interfere with the identification/determination of HGA. 6 Apparatus Usual laboratory equipment, glassware, and the following: 6.1 Magnetic stirrer. 6.2 Chromatograph, equipped with: a) an isocratic pump delivering the eluent at a flow rate of 1 ml/min; b) an injection valve with a 20
c) a NH2 column; internal diameter: 4,6 mm; column length: 250 mm; dp = 5 1); d) a NH2 guard-column (recommended); e) a UV-Vis detector with a 210 nm-filter; f) an integrator. 6.3 Chromatographic conditions, according to Table 1. Table 1 — Chromatographic conditions Flow rate Eluent A (7.4) % Eluent B (7.5) % 1 ml/min 75 25 6.4 Balance, Balance, with an accuracy of ± 0,1 mg. 6.5 Membrane filters. Micro membrane filters resistant to aqueous solutions, with porosity of respectively 0,45 0,2
7 Reagents Use only reagents of recognized analytical grade.
1) Phenosphere NH2 80A 5 µm 250×4,6 mm or equivalent. This is an example of 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 of this product. Equivalent products can be used if they can be shown to lead to the same results.
SIST EN 16847:2016
EN 16847:2016 (E) 6 7.1 Water, conforming to EN ISO 3696, degassed by boiling before use. 7.2 Sample preparation solvent. Add to 800 ml of water, 2 ml of ortho-phosphoric acid 85 % and 25 ml of methanol in a 1 l volumetric flask. Dilute to the mark with water and homogenize. 7.3 HGA stock solution, c(HGAacid) = 19 893 mg/l. This solution shall be freshly prepared daily, because of the formation of the corresponding lactone if it let standing for a long period of time. Weigh to an accuracy of 0,1 mg about 2 500 mg of the heptagluconic acid, sodium salt dihydrate (CAS # 10094-62-9), c > 99 %, add 50 ml of water in a 100 ml volumetric flask. After dissolution, dilute to the mark with water and homogenize. 7.4 Eluent A: ortho-phosphoric
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