🍎 Determination of arsenic, cadmium, cobalt, copper, iron, mercury, manganese, molybdenum, lead, selenium, thallium, uranium and zinc in animal feed by ICP-MS after pressure digestion with concentrated nitric acid (≥ 210 °C, also microwave with hydrogen peroxide); extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite) after boiling with diluted nitric acid; external calibration or standard addition, internal standard (rhodium), protection of mercury against adsorption (HCl or gold); limits of quantification usually 0.03–5.0 mg/kg; PN-EN 17053:2018-03

Food chemistry PN-EN 17053

Overview

WHAT THE STANDARD COVERS. We read the text of the standard in the iTeh sample of SIST EN 17053:2018 (Slovenian adoption of EN 17053:2018 of January 2018, English text) — PN-EN 17053:2018-03 adopts EN 17053:2018 as identical (PKN search): European foreword, Clauses 1–7 and Clause 8 up to 8.5.3 with Table 1 — the sample ends on page 10. We do not read the rest of the determination, calculation, precision, test report or Annexes A (interlaboratory study data) and B (interferences and techniques for reducing them); we know their titles and role from the text of the clauses.

ACCORDING TO THE TEXT OF EN 17053:2018. The standard was prepared by CEN/TC 327 “Animal feeding stuffs — Methods of sampling and analysis” (secretariat NEN) under a mandate of the European Commission and EFTA; CEN approved it on 27.11.2017, national adoption by July 2018 at the latest. Warning: the method involves reagents hazardous to health. Scope (1): determination of trace elements, heavy metals and other elements in animal feed by ICP-MS — As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the solution after pressure digestion; extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) — wet digestion with nitric acid; quadrupole instruments with or without molecular interference reduction techniques, and high-resolution sector-field systems; the method was statistically tested in a collaborative trial on eight feed samples; for elements with HORRAT above 2 (e.g. mercury, Annex A) the method is more applicable as a screening method than for confirmatory purposes; high-resolution ICP-MS was not tested in validation; the limit of quantification depends on matrix and instrument — normally 0.10 mg/kg for Co, Mn, Mo, Pb, Tl, U, 5.0 mg/kg for Fe and Zn, 0.03 mg/kg for Cd, 0.04 mg/kg for Hg and 0.05 mg/kg for As. References (2): EN ISO 3696 (water), EN ISO 6498 (preparation of feed samples). Principle (3): digestion of a test portion with concentrated nitric acid under pressure; for extractable lead — wet digestion with nitric acid; determination by ICP-MS with external calibration or standard addition; mass interferences are reduced by mathematical correction equations, physical or chemical solutions or high-resolution ICP-MS. Reagents (4): water grade 2 according to EN ISO 3696; nitric acid ≥ 65 % (14.4 mol/l); 5 % solution (54 ml to 1000 ml); rinsing solution (20 ml to 1000 ml); hydrochloric acid 30 %; hydrogen peroxide ≥ 30 %; stock solutions 1000 mg/l (certified multi-element ones advisable, stable for several months); calibration solutions prepared daily, checking chemical compatibility and purity when mixing single-element ones; internal standard — rhodium recommended (alternatively germanium, indium or scandium for low masses; rhenium, thulium, lutetium for high masses), working solution 1 mg/l; gold chloride (10 g Au/l) and gold stability solution 200 mg Au/l. Apparatus (5): grinders to ≤ 0.5 mm (e.g. knife mill) and ≤ 0.1 mm (e.g. ball mill), checking that they do not change element content (adsorption, contamination); balance 1 mg; pressure digestion apparatus above 210 °C (instead of PTFE vials better quartz, FEP or PFA; quartz above 230 °C), optionally microwave; ICP-MS; freeze-dryer for liquid feeds; oven 70 ± 5 °C; 250 ml beakers; hot plate. Sampling (6): not part of the method — EN ISO 6497 recommended; the sample must be representative and unchanged in transport. Preparation (7): according to EN ISO 6498 — grinding without heating and without contamination from tools, quickly (so as not to change water content), in a closable container (e.g. polypropylene), thorough mixing — the test portion is at most 0.5 g; feeds — approx. 500 g ground to ≤ 0.5 mm; mineral feeds to ≤ 0.1 mm, but products with crystalline water (e.g. MgCl2·6H2O, phyllosilicates) are not ground. Procedure (8): pressure digestion — e.g. 0.5 g, 3 ml HNO3, 30 min pre-digestion, to 150 °C in 60 min, to ≥ 210 °C in 40 min, 90 min; microwave — 0.5 g, 3 ml HNO3 and 0.5 ml H2O2, ≥ 210 °C for ≥ 20 min; blank treated alike; extractable lead — 2 g with 85 ml of 5 % HNO3, boiled 30 min under a watch-glass, to 100 ml, filtered; external calibration — at least five solutions recommended (including a blank), after proving linearity a two-point calibration is allowed, matrix matching at least in acid composition and concentration; standard addition — at least four points (three additions), near the LOQ three points, highest addition 3 to 5 times the sample concentration; measuring solutions diluted to a salt content < 0.2 % (for HR-ICP-MS e.g. ≤ 0.05 %), internal standard at equal concentration (e.g. 10 µg/l, for HR-ICP-MS e.g. 1 µg/l); mercury — against adsorption and memory effects HCl to 0.5–1 % or gold at least 0.2 mg Au/l in all solutions; optimization — oxides and doubly charged ions below 3 %, rinsing the nebulizer, checking rinse time on a blank; Table 1 — isotopes (e.g. 75As, 111/112/114Cd, 59Co, 63/65Cu, 56Fe, 201Hg, 55Mn, 95Mo, 206/207/208Pb summed, 78/80/82Se, 205Tl, 238U, 66/68Zn), isobaric and molecular interferences (e.g. 40Ar35Cl+ for 75As, 40Ar16O+ for 56Fe) and techniques: mathematical correction, KED, reaction mode.

STATUS (as of 03.10.2026). The PKN search engine (query “PN-EN 17053”, 03.10.2026) lists PN-EN 17053:2018-03 in Polish and English versions, “Introduces: EN 17053:2018 [IDT]”, without a withdrawal note.

HOW MANY LABORATORIES AND IN WHAT FORM (copy of the accreditation scope database, data up to 17.09.2026, read 03.10.2026). The number 17053 appears in 2 records at 2 laboratories: AB 381 and AB 545. In the current PCA documents (read 03.10.2026; AB 545 issue no. 25 of 31.10.2025, AB 381 issue no. 29 of 10.06.2026) the number appears at the same 2 laboratories; in every document the number of page markers equals the number of PDF pages, without repetitions; a search of all PCA documents downloaded from BIP on 03.10.2026 found no laboratories outside the database copy. The form “PN-EN 17053:2018-03” at AB 545, “PN-EN 17053” without year at AB 381. None of these items is suspended. The “Laboratories” tab (query “PN-EN 17053”) shows both laboratories — checked by a tab query on the labcoda.pl production server on 03.10.2026.

WHAT THE LABORATORIES TEST (items in PCA). AB 545: feeds — selenium (0.20–200) mg/kg, molybdenum (0.50–4.00), cobalt (0.20–105), lead (0.020–10.0), cadmium (0.040–10.0), arsenic (0.20–30.0), mercury (0.002–0.60) mg/kg; ICP-MS. AB 381: feeds — content of elements by ICP-MS, without a list of elements and ranges in the item.

WHERE A SEEMINGLY CORRECT RESULT IS EASY TO GET. Mercury: for elements with HORRAT above 2 (e.g. mercury) the method is more applicable for screening than for confirmation (1); without added HCl or gold mercury adsorbs and gives memory effects (8.4.2); the usual LOQ for mercury is 0.04 mg/kg, while the AB 545 item starts at 0.002 mg/kg — such a range requires confirmation in the laboratory’s procedure. Lead in minerals: for minerals and feeds with phyllosilicates extractable lead after boiling with diluted acid is determined, not total lead after pressure digestion — these are different quantities (1, 3, 8.2). Grinding: the mill may introduce or adsorb elements, heating changes water content, and products with crystalline water are not ground (5.1, 7). Test portion: at most 0.5 g, so sample inhomogeneity passes directly into the result (7.1). Calibration: two-point calibration only after proving linearity, and matching the acid in calibration solutions is mandatory (8.3.2). Interferences: e.g. 40Ar35Cl+ on 75As or 40Ar16O+ on 56Fe — without correction, KED or reaction mode the result rises (Table 1). Salt: a salt content above 0.2 % in the measuring solution disturbs the measurement (8.4.1). High-resolution ICP-MS: it was not covered by the validation (1).

WHAT WE DO NOT GIVE. We do not quote the calculations, precision data of the interlaboratory study, the tested working ranges for individual elements or the description of interference reduction techniques of Annex B — they lie outside the sample. We do not summarize EN ISO 6497, EN ISO 6498 or EN ISO 3696 in this entry. We do not give maximum contents of undesirable substances in feed.

Method principle

A portion of ground feed is digested with concentrated nitric acid in a closed vessel under pressure at not less than 210 °C (in minerals with phyllosilicates lead is extracted by boiling with diluted nitric acid). The solution is diluted, an internal standard is added and it is measured in an inductively coupled plasma mass spectrometer: elements are ionized in the plasma, and ions of selected isotopes are separated by mass-to-charge ratio. Concentrations are calculated by external calibration or standard addition, limiting interferences by mathematical correction, collision cell (KED) or reaction mode.

Applications

• As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in animal feed — multi-element method (1)
• Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite) (1, 8.2)
• Mineral feeds and liquid feeds — sample preparation according to EN ISO 6498 (5, 7)
• Feeds — selenium, molybdenum, cobalt, lead, cadmium, arsenic, mercury — 2 accreditation scope records of 2 laboratories in PCA

Key parameters

Standard

Standard number

PN-EN 17053:2018-03

Title (PL)

Pasze: Metody pobierania próbek i analiz — Oznaczanie pierwiastków śladowych, metali ciężkich i innych pierwiastków w paszy metodą ICP-MS (metoda wielopierwiastkowa)

Title (EN)

Animal feeding stuffs: Methods of sampling and analysis — Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method)

Step-by-step procedure

1. Sample preparation

   According to EN ISO 6498: grinding to ≤ 0.5 mm (mineral ≤ 0.1 mm), without heating and contamination (7). PN-EN 17053:2018-03 — no withdrawal note (PKN, 03.10.2026).

2. Digestion

   Pressure digestion with HNO3 (≥ 210 °C) or lead extraction with 5 % HNO3 for minerals with phyllosilicates; blank (8.1, 8.2).

3. Measuring solutions

   Dilution to salt < 0.2 %, internal standard, HCl or Au for mercury (8.4).

4. ICP-MS measurement

   Optimization (oxides < 3 %), isotopes and techniques of Table 1 (8.5).

5. Calibration and result

   External calibration (≥ 5 points) or standard addition (≥ 4 points) (8.3; calculations outside the sample).

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• The method involves reagents hazardous to health (concentrated acids, hydrogen peroxide); the user is responsible for protective measures (foreword, 4)
• Pressure digestion — the sample mass is matched to the vessel capacity, strictly following the manufacturer’s instructions (8.1.1)

Frequently asked questions