EN 15905-2010 pdf download.Fertilizers – Determination of 3-methylpyrazole (MP) using highperformance liquid chromatography (HPLC).
This EN 15905 specifies a method for the determination of the 3-methylpyrazole (MP) content in fertilizers, in particular in urea and materials containing urea using high-performance liquid chromatography
(HPLC).
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 impro vers — Vocabulary — Part 1: General terms
EN 12944-2:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 2: Terms relating to fertilizers1) (Including corrigendum AC:2000)
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 Principle
The sample of fertilizer is dissolved in water or extracted with water. The 3-methlypyrazole is determined in the solution using reversed phase high-performance liquid chromatography with an UV detector,
5 Reagents
Use only reagents of recognized analytical grade and distilled or demineralized water (grade 3 according to
EN ISO 3696:1995).
5.1 Acetonitrlle, HPLC punty.
5.2 De-ionized water, conductivity less than 0,5 mS/rn according to ISO 3696, grade 3.
6.5 Volumetric flasks,100 ml, 1 000 ml.
6.6 HPLC device, for socratic working procedure.
6.7’ Sample issuing system.
6.8 UV detector.
6.9 Evaluation unit, e.g. electronic integrator.
6.10 Reversed phase HPLC separator column, e.g. C18 10 im, 250 mm x 4 mm.
NOTE With suitable separation performance, it is also possible to use a shorter separation column. Instead of a C18
column, a separation column with hydroxyt phase can be used.
7 Sampling and sample preparation
Sampling is not part of the method specified in this document. A recommended sampling method is given in
EN 1482-1.
Sample preparation shall be carried out in accordance with EN 1482-2.
8 Procedure
8.1 PreparatIon of the test solution
Weigh a test portion corresponding to approximately 8 mg of 3-methlypyrazole into a 1 000 ml volumetric flask. Add approximately 750 ml of water (5.2) and dissolve in the ultrasonic bath (6.2). Make up to the mark with water (5.2) and filter a part of the sample solution through a membrane filter (6.3, 6.4) in order to remove any un-dissolved substances which may still be present. This solution is used for the determination.
NOTE The amount of ammonium nitrate-urea solution weighed in is 10 g. precise to 10 mg, For solid fertilizers, for reasons of homogeneity, an amount weighed in should be used of 100 g, precise to 0,1 g. In this case, the dilution of the filtrate by 1+9 is necessary; this is to be taken into account during the calculation
8.2 Preparation of the calibration solutions
Weigh I g of 3-methylpyrazole (5.3) to the nearest of 0,1 mg into a 1 000 ml volumetnc flask. Dissolve with water (5.2), make up to the mark with water (5.2) and mix well. Pipette 10 ml of this solution into a 100 ml volumetric flask, make up to the mark with water (5.2) and mix well. Pipette 5 ml, 10 ml, and 15 ml of this solution into three 100 ml volumetric flasks, Make up each flask to the mark with water (5.2) and mix well. Take the solutions to create the calibration curve.
10 Precision
10.1 Inter-laboratory test
An inter-laboratory test has been carried out in 2008 with 9 participating laboratories and 2 different samples of fertilizers. This test yielded the data given in Annex A. Repeatability and reproducibility were calculated according to ISO 5725-1 and ISO 5725-2.
The values derived from this inter-laboratory test may not be applicable to concentration ranges and matrices other than those given in Annex A.
10.2 Repeatability
The absolute difference between two independent single test results, obtained with the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, will in not more than 5 % of the cases exceed the values of r given In Table 1.
10.3 Reproducibility
The absolute difference between two single test results, obtained with the same method on identical test material in different laboratories by different operators using different equipment, will in not more than 5 % of the cases exceed the values of R given in Table 1.EN 15905-2010 pdf download.
EN 15905-2010 pdf download
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