CEN/TC 260/WG 7 - Chemical analysis

This document specifies a method for the determination of methylen-urea (MU) oligomers in inorganic fertilizers using high-performance liquid chromatography (HPLC).
The method is applicable to all fertilizers which do not contain interfering organic compounds.
NOTE   By the condensation of urea and formaldehyde, several oligomers are formed, such as methylen-diurea (MDU), dimethylen-triurea (DMTU), trimethylen-tetraurea (TMTU) and higher oligomers. The three molecules named here are the most soluble in water, while the higher compounds are insoluble in hot water, but their nitrogen is available for plants by microbiological decomposition. Also, urea is always a companion of MU-oligomers.

This document specifies a method for the determination of nitrogen content in IBDU (isobutylidenediurea) and CDU (crotonylidenediurea) using high-performance liquid chromatography (HPLC).
The method is applicable to all fertilizers which do not contain interfering organic compounds.

This document specifies a method for the determination of phosphorus in fertilizer extracts.
The method is applicable to all extracts of fertilizers for the determination of the different forms of phosphorus as phosphorus soluble in mineral acids, water-soluble phosphorus, phosphorus soluble in solutions of neutral ammonium citrate, phosphorus soluble in 2 % citric acid and phosphorus soluble in a mass fraction of 2 % formic acid.
The method has only been validated on inorganic fertilizers but can be applicable to all extracted phosphorous if proper extraction methods are used.

This document specifies a method for the determination of total nitrogen in nitrate-free calcium cyanamide.

This document specifies a method for the determination of cyanamide nitrogen in fertilizers. The method is applicable to calcium cyanamide and mixtures of calcium cyanamide with calcium nitrate.

This document specifies a method for the determination of total nitrogen in calcium cyanamide. The method is applicable to calcium cyanamide containing nitrates.

This document specifies three different methods (Methods A, B and C) for the determination of sulfur present in fertilizer 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).

This document specifies references to methods for the determination of the content of the following specific nutrients in inorganic fertilizers:
-   the total nitrogen content;
-   the ammoniacal nitrogen content;
-   the nitric nitrogen content;
-   the urea nitrogen content;
-   the content of nitrogen from isobutylidenediurea (IBDU) and crotonylidenediurea (CDU);
-   the cyanamide nitrogen content;
-   the methylene-urea nitrogen content (and urea formaldehyde, if applicable);
-   the total phosphorus content;
-   the water-soluble phosphorus content;
-   the neutral ammonium citrate soluble phosphorus content;
-   the water-soluble potassium content;
-   the total magnesium content;
-   the water-soluble magnesium content;
-   the total calcium content;
-   the water-soluble calcium content;
-   the total sulfur content;
-   the water-soluble sulfur content;
-   the total sodium content;
-   the water-soluble sodium content.
This document is applicable to EU fertilizing products classified as PFC 1(C) and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1(C), PFC 2 and PFC 5 as specified in the Regulation (EU) 2019/1009 [1].

This document specifies a method for the determination of the chloride content in organic fertilizers, organo-mineral fertilizers, inorganic fertilizers and liming materials by potentiometric titration.

This document specifies a method for the determination of the chloride content in ammonium nitrate fertilizers of high nitrogen content.

This document specifies a method for the determination of pH of a solution of ammonium nitrate fertilizers of high nitrogen content.

This document specifies references to methods for the determination of the content of the following specific micronutrients in inorganic fertilizers:
-   the total boron content;
-   the total cobalt content;
-   the total copper and zinc content;
-   the total iron content;
-   the total manganese content;
-   total molybdenum content;
-   the water-soluble boron content;
-   the water-soluble cobalt content;
-   the water-soluble copper content;
-   the water-soluble iron content;
-   the water-soluble manganese content;
-   the water-soluble molybdenum content;
-   the water-soluble zinc content;
-   the sum of declared micronutrients in compound micronutrient fertilizers.
This document is applicable to EU fertilizing products classified as PFC 1(C) and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1(C), PFC 2 and PFC 5 as specified in the Regulation (EU) 2019/1009 [2].
An overview of the references to methods for the determination of the specific micronutrients is given in Table 1.

This document specifies references to the methods for the determination of nitrification inhibitors and urease inhibitors in inorganic fertilizers.
This document is applicable to EU fertilizing products classified as PFC 1(C) and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1(C), PFC 2 and PFC 5 as specified in the Regulation (EU) 2019/1009 [1].

This document specifies a method for the determination of particle size of ammonium nitrate fertilizers of high nitrogen content.

This document specifies references to a method for the determination of the chloride content in organic fertilizers, organo-mineral fertilizers, inorganic fertilizers and liming materials.
This document is applicable to EU fertilizing products classified as PFC 1, PFC 2 and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1, PFC 2 and PFC 5 as specified in the Regulation (EU) 2019/1009 [1].

This document specifies references to methods for the determination of the following specific parameters in ammonium nitrate fertilizers of high nitrogen content:
-   the nitrogen content as a result of ammonium nitrate;
-   pH of a solution of ammonium nitrate fertilizers of high nitrogen content;
-   the particle size of ammonium nitrate fertilizers of high nitrogen content;
-   the chloride content;
-   the copper content.
This document is applicable to EU fertilizing products classified as PFC 1(C)(I)(a)(i-ii)(A) and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1(C), PFC 2 and PFC 5 and still fulfils the requirements for PFC 1(C)(I)(a)(i-ii)(A) as specified in the Regulation (EU) 2019/1009 [1].

This document specifies a reference to the method for the determination of the granulometry.
This document is applicable to solid inorganic macronutrient fertilizers classified as PFC 1(C)(I)(a) and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1(C)(I)(a) and PFC 5 as specified in the Regulation (EU) 2019/1009 [1].

This document specifies a method for the determination of the copper content in ammonium nitrate fertilizers of high nitrogen content.

This document specifies references to methods for the determination of the following contaminants: mercury, cadmium, nickel, copper, zinc, arsenic, lead, chromium (VI), biuret, perchlorate and total chromium content in inorganic fertilizers.
This document is applicable to EU fertilizing products classified as PFC 1(C) and PFC 7 as long as the blend only consists of EU fertilizing products classified as PFC 1(C), PFC 2 and PFC 5 as specified in the Regulation (EU) 2019/1009 [3].
An overview of the references to methods for the determination of the specific contaminants is given in Table 1.
NOTE 1   The determination of copper and zinc in inorganic fertilizers as micronutrients is covered by CEN/TS 17754:2022.
NOTE 2   The determination of copper in ammonium nitrate fertilizers of high nitrogen content is covered by CEN/TS 17751:2022.

This document specifies a method for the determination of traces of perchlorate by liquid chromatography and tandem mass spectrometry detection (LC-MS/MS). The method is applicable to mineral fertilizers.

This document specifies a method for the determination of the cold and hot water insoluble nitrogen content in solid urea formaldehyde and methylene urea slow-release fertilizers and for the determination of the solubility of nutrient polymers in a phosphate buffer solution with a pH of 7,5 at 100 °C.

This document specifies a method for the determination of traces of perchlorate in mineral fertilizers by ion chromatography and conductivity detection (IC-CD).

This document specifies a method for the determination of nitrification inhibitor 2-(3,4-dimethyl-pyrazol-1-yl)-succinic acid (DMPSA) using high-performance liquid chromatography (HPLC), which is applicable to all mineral fertilizers.

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing less than or equal to 10 % boron. The method is not suitable for fertilizers with Fe concentrations more than twenty times higher than the concentration of boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
The method can also be used for the determination of boron in mineral fertilizers containing more than 10 % boron after appropriate dilution of the extracts.

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing more than 10 % boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
NOTE   A method used for the determination of boron in mineral fertilizers containing less than or equal to 10 % of boron (spectrophotometric determination by azomethine-H) can be also used for the scope of this method after appropriate dilution of the extracts.

This European Standard specifies a method for determination of total and water extractable molybdenum in mineral fertilizers containing less than or equal to 10 % molybdenum.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.

This European Standard specifies a method for the determination of cobalt, copper, iron, manganese and zinc in fertilizer extracts using flame atomic absorption spectrometry (FAAS).
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by FAAS and it is not necessary to apply organic matter removal.

This European Standard specifies a method for the determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc in fertilizer extracts using inductively coupled plasma-atomic emission spectrometry (ICP-AES).
This method is applicable to water and aqua regia fertilizer extracts prepared according to EN 16962 and/or EN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by ICP-AES and it is not necessary to apply organic matter removal.

This European Standard specifies a method for the extraction of water soluble forms of boron, cobalt, copper, iron, manganese, molybdenum and zinc from mineral fertilizers containing one or more micro-nutrients and the procedure for removal of organic compounds from the water extracts.
The extracts can be analysed according to EN 16963, EN 16965, prEN 17041, prEN 17042, prEN 17043 and CEN/TS 17060.

This European Standard specifies a method for the total extraction of boron, cobalt, copper, iron, manganese, molybdenum and zinc with aqua regia from mineral fertilizers containing one or more micro-nutrients.
The extracts can be analysed according to EN 16963, EN 16965, prEN 17041, prEN 17042 and prEN 17043.
This method is also suitable for the extraction of cadmium, chromium, nickel and lead to be determined according to EN 16319; the extraction of mercury to be determined according to EN 16320 and the extraction of arsenic to be determined according to EN 16317.

This European Standard specifies a method for the extraction of water-soluble calcium, magnesium, sodium and sulfur (in the form of sulfates), so that the same extract can be used for the determination of each nutrient required.
The method is solely applicable to fertilizers listed in Regulation (EC) 2003/2003, Annex I [2]), for which a declaration of the water-soluble calcium, magnesium, sodium, and sulfur (in the form of sulfates) is provided for in this Regulation.

This Technical Specification specifies the procedure for determination of total and water extractable molybdenum in mineral fertilizers containing more than 10 % molybdenum. This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 260172 and/or EN 260176.

This European Standard specifies a method for the determination of the content of cadmium, chromium, nickel and lead in fertilizers with inductively coupled plasma atomic emission spectrometry (ICP-AES) after extraction with aqua regia. Limits of quantification are dependent on the sample matrix as well as on the instrument, but can roughly be expected to be 0,3 mg/kg for Cd and 1 mg/kg for Cr, Ni and Pb.
NOTE   Due to significant interference from Cu, Fe and Mn, no valid results can be reported using this method for fertilizer matrices containing high concentrations (>/= 10 %) of these micro-nutrients.

This European Standard specifies a method for the quantitative determination of the urease inhibitors N-(n-Butyl)thiophosphoric acid triamide (NBPT, CAS-No. 94317-64-3) and N-(n-Propyl)thiophosphoric acid triamide (NPPT, CAS-No. 916809-14-8) content in urea based fertilizers using high-performance liquid chromatography (HPLC).

This European Standard specifies a method for the determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP, CAS-No: 202842-98-6) in mineral N containing fertilizers using high-performance liquid chromatography (HPLC).

This European Standard specifies a method for the determination of magnesium in fertilizer extracts by complexometry.
The method is applicable to the following EC fertilizer extracts for which the determination of total magnesium and/or water-soluble magnesium is provided for according to the Regulation (EC) No 2003/2003, Annex I [3]:
- fertilizers listed in [3], Annex I: straight nitrogenous fertilizers, type 1b + 1c (calcium magnesium nitrate), type 7 (magnesium sulfonitrate), type 8 (nitrogenous fertilizers with magnesium) and straight potassic fertilizers, type 2 (enriched kainite), type 4 (potassium chloride containing magnesium), type 6 (potassium sulfate containing magnesium salt);
- fertilizers listed in [3], Annex I D relating to secondary nutrients.

This European Standard specifies a method for the determination of the magnesium content in fertilizer extracts using atomic absorption spectrometry (AAS).
This method is applicable to EC fertilizer extracts obtained according to EN 15960 and EN 15961, for which a declaration of the total magnesium and/or water soluble magnesium content is required, with the exceptions of the following fertilizers according to [4], Annex I D relating to secondary nutrients:
- type 4 (kieserite);
- type 5 (magnesium sulfate) and type 5.1 (magnesium sulfate solution);
- type 7 (kieserite with potassium sulfate)
to which [4], method 8.8, applies.
NOTE   Method 8.8 is covered by CEN/TS 16198 [2].
The method applies to all fertilizer extracts containing elements in quantities that might interfere with the complexometric determination of magnesium.

This European Standard specifies a method for the determination of the sodium content in fertilizer extracts by flame-emission spectrometry.
The method is applicable to EC fertilizers for which a declaration of the sodium content is provided for in Regulation (EC) Nr 2003/2003, Annex I [3].

This European Standard specifies a manganimetric method for the determination of the calcium content in fertilizer extracts.
This method is applicable to EC fertilizers for which a declaration of the total and/or water-soluble calcium content is provided for in Regulation (EC) No 2003/2003, Annex I [3].

This European Standard specifies a method for the determination of chlorides in the absence of organic material. The method is applicable to all fertilizers which are free from organic material.

In Regulation (EC) No. 2003/2003 [2] tolerance limits are mentioned for nutrient contents in mineral fertilizers (Annex II of Regulation (EC) No. 2003/2003) as well as prescribed methods for control purposes (Annex IV of Regulation (EC) No. 2003/2003).
Prior to the work done by CEN/TC 260 following Mandate M/335, no statistical data were available for the official analytical methods to be applied. Due to the standardization work done for this mandate, statistical data have been generated as ring testing was a major topic in this mandate.
This Technical Specification describes to what extent the presently applied tolerances are in line with the obtained precision data from the analytical methods studied.
The purpose of this document is to give feedback on the applied tolerances within Regulation (EC) No. 2003/2003 based on the method evaluation done as an outcome of the work executed by CEN/TC 260/WG 7 according to Mandate M/335. This evaluation of the tolerances was part of Mandate M/418.

This European Standard specifies a method for extraction and determination of the elemental sulfur contained in fertilizers.
The method is applicable to EC fertilizers for which a declaration of the total sulfur in elemental form is provided for in Regulation (EC) Nr 2003/2003, Annex I [1].

This European Standard specifies a method for the extraction of water soluble phosphorus.
The method is applicable to all fertilizers, including compound fertilizers, where water soluble phosphorus is to be determined.

This European Standard specifies a method for the extraction of total calcium, total magnesium and total sodium and for the extraction of total sulfur present in the form of sulfates, so that the same extract may be used for the determination of each nutrient required.
The method is applicable to fertilizers listed in Regulation (EC) 2003/2003, Annex I [2], for which a declaration of total calcium, total magnesium, total sodium, and total sulfur in the form of sulfates is provided for in this Regulation.

This European Standard specifies a method for the determination of N-(2-nitrophenyl)phosphoric triamide (2-NPT) in urea or in fertilizers containing urea using high-performance liquid chromatography (HPLC).

This document specifies a method for the determination of phosphorus soluble in mineral acids.
The method is applicable exclusively to phosphate fertilizers listed in Regulation (EC) 2003/2003, Annex I (see [2]).

This document specifies a method for the extraction of the total sulfur contained in fertilizers in elemental form and/or in other chemical combinations.
The method is applicable to EC fertilizers for which a declaration of the total sulfur present in various forms (elemental, thiosulfate, sulfite, sulfate) is provided.

This document specifies a method for the determination of the fineness of grinding of soft natural phosphates by wet sieving.

This document specifies a method for the extraction of water-soluble sulfur contained in fertilizers in various forms.
The method is applicable to EC-fertilizers for which a declaration of the water-soluble sulfur trioxide is provided for.

This document specifies a method for the extraction of phosphorus soluble in neutral ammonium citrate.
The method is applicable to all fertilizers in respect of which solubility in neutral ammonium citrate is laid down in Regulation (EC) 2003/2003, Annex I (see [2]).