BS EN 17053:2018 pdf download.Animal feeding stuffs: Methods of sampling and analysis – Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method)
1 Scope
This European Standard specifies a method for the determination of trace elements, heavy metals and other elements in animal feed by inductively coupled plasma mass spectrometry ([ICP-MS). The method is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, TI, U and Zn in the extraction solution after pressurized digestion. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described is suitable for use in quadrupole instruments equipped either with or without additional technology to reduce molecular ion interferences [e.g. collision or reaction technologies) as well as in high-resolution sector-field systems. The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, TI, U and Zn. For elements with a HORRAT value higher than 2 [e.g. mercury, see Annex A) the method is more applicable as a screening method and not for confirmatory purposes. High-resolution sector-field ICP-MS was not tested in the validation ring trial. The limit of quantification for each element is dependent on the sample matrix as well as the instrument. For the elements Co, Mn, Mo, Pb, TI, U a limit of quantification of 0,10 mg/kg should normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg and As 0,05 mg/kg should normally be quantifiable. Details on the successfully tested working range for each element are described in this standard.
8.1 Pressure digestion
8.1.1 General
Match the initial sample mass to the capacity of the digestion vessel, with the manufacturer’s instructions being strictly followed for safety reasons.
8.1.2 Example of a high pressure digestion
When using a 100 ml vial, weigh about 0,5 g of the prepared test sample to the nearest 1 mg. Add 3 ml of nitric acid (4.1) and seal the digestion vial and the pressure vial in the correct manner. Leave to pre- digest for about 30 min and heat it in a pressure digestion apparatus (5.3) from room temperature to 150。C in 60 min, then to at least 210 °C in 40 min and keep this temperature for 90 min before cooling down. Dilute the digestion solution accordingly with water. Treat a blank in the same way. 8.1.3 Example of microwave digestion When using 100 ml vials, weigh about 0,5 g of the prepared test sample to the nearest 1 mg. Add 3 ml of nitric acid (4.1) and 0,5 ml of hydrogen peroxide [4.5), seal the digestion vial and the pressure holders in the correct manner. Leave to pre-digest outside the microwave oven (5.3) for about 30 min. Apply low microwave energy at the beginning of the digestion and slowly raise the energy to the maximum power, to reach at least 210 °C. Hold this temperature for at least 20 min, cool down for minimum 20 min to 25 min. Dilute the digestion solution accordingly with water. Treat a blank in the same way.
BS EN 17053:2018 pdf download
