🍎 Determination of lead, cadmium, chromium and molybdenum in food by graphite furnace atomic absorption spectrometry (GFAAS) — solution after pressure digestion according to EN 13805 without further treatment, spectrometer with background correction (Zeeman recommended) and pyrolytically coated tubes with or without a L'vov platform, modifiers (magnesium nitrate, palladium with magnesium nitrate, ammonium phosphate with magnesium nitrate, palladium with ascorbic acid), wavelengths Pb 283,3 nm, Cd 228,8 nm, Cr 357,9 nm, Mo 313,3 nm; calibration or standard addition, blanks and reference materials in every series; result in mg/kg, PN-EN 14083

Food chemistry PN-EN 14083

Overview

WHAT THE STANDARD COVERS. We read the text of the standard in the iTeh sample of SIST EN 14083:2003, i.e. EN 14083:2003 (English text): contents, foreword, Clauses 1–7 and the beginning of Clause 8 (limit of quantification) — the sample ends on page 7, before Table 2. We do not read Table 2 (required quantifiable concentrations), precision (9), the test report (10) or Annex A (results of the interlaboratory test); we know the titles from the contents.

ACCORDING TO THE TEXT OF EN 14083:2003. The standard was prepared by CEN/TC 275 “Food analysis — Horizontal methods” (secretariat DIN); approved by CEN on 18.12.2002; national standards had to adopt it, and withdraw conflicting ones, by October 2003 at the latest; Annex A is informative. Scope (1): determination of lead, cadmium, chromium and molybdenum in foodstuffs by GFAAS after pressure digestion; foodstuffs for which specific European standards exist are excluded from the scope of this horizontal standard — the analyst shall review whether vertical standards exist. References (2): EN 13804 (performance criteria, general considerations, sample preparation), EN 13805 (pressure digestion). Principle (3): determination of the elements in the test solution by GFAAS after pressure digestion according to EN 13805; warning: the standard does not address all safety problems. Reagents (4): the trace element content of reagents and water must be low enough not to affect the result; HCl not less than 25 % (≈ 1,13 g/ml) and HNO3 not less than 65 % (≈ 1,4 g/ml), suitable for trace analysis; stock solutions 1000 mg/l — certified ones advisable; as an example: Pb — 1,598 g Pb(NO3)2 in HNO3 1 %, Cd — 1,000 g cadmium metal in HCl 1 %, Cr — 3,735 g K2CrO4 in water, Mo — 1,840 g ammonium heptamolybdate in 1 % ammonia solution; calibration solutions within the linear range, at least 3 recommended, with acid concentration as in the test solution; zero member solutions with water and acid as in the test solution; modifiers — examples may vary considerably in composition and concentration, the starting point for optimization is the instrument manufacturer’s recommendation: magnesium nitrate (0,25 g Mg(NO3)2·6H2O in 100 ml), palladium with magnesium nitrate (0,075 g Pd in HNO3, 0,05 g magnesium nitrate, to 50 ml), ammonium dihydrogen phosphate with magnesium nitrate (0,5 g and 0,05 g, 1 ml HNO3, to 50 ml), palladium with ascorbic acid (solutions A and B 1:1); commercial magnesium nitrate and palladium solutions may be used; note: the modifier for a given element is applied already when establishing the optimum furnace temperature programme. Apparatus (5): equipment in contact with the sample is prepared according to EN 13804; spectrometer with background correction (Zeeman recommended), argon-supplied graphite furnace and recording; pyrolytically coated tubes with or without a L’vov platform (recommendation); autosampler; hollow-cathode or electrodeless discharge lamps for Pb, Cd, Cr and Mo. Procedure (6): the solution after digestion according to EN 13805 may be measured without further treatment; before each determination the instrument is set according to the manual and the programme established (preferably with the sample matrix) — decomposition and atomization temperatures and times, matrix modification, injection volumes; Table 1 (example): hollow-cathode lamp, Pb 283,3 nm, Cd 228,8 nm, Cr 357,9 nm, Mo 313,3 nm, slit 0,7 nm; the calibration method may be used if the slope of the calibration function does not differ significantly from the slope in the standard addition method; interferences are reduced by modifiers with the L’vov platform; with a platform, peak area measurement is recommended; calibration: zero on the zero member solution, a function for each element, linear range determined and regularly checked, solutions above it diluted, in long series zero member and selected calibration solutions are checked; standard addition: within the linear range, at least three points including two additions, the highest 3–5 times the concentration in the sample, the lower one half of the highest, extrapolation to the concentration axis; with addition directly into the furnace without dilution the risk of contamination is much smaller; quality control (6.3): in each series blanks and reference samples of reliably known content according to EN 13804, carried through all steps from digestion. Calculation (7): content in mg/kg from w = a · V · F / m (a — concentration in the test solution in mg/l, V — volume of the digestion solution in ml, F — dilution factor, m — sample mass in g), with blank subtracted if necessary. Limit of quantification (8): the spectrometer shall be able to determine the concentrations of Table 2 with an injection of 20 µl of measuring solution (table values outside the sample).

STATUS (as of 03.10.2026). In the PKN search (term “14083”, 03.10.2026) PN-EN 14083:2004 (Polish version, “Introduces: EN 14083:2003 [IDT]”) has no withdrawal note; PN-EN 14083:2003 (English version) has the note “Withdrawn and replaced by PN-EN 14083:2004 – Polish version”; the third result, PN-EN ISO 14083:2023-10, is an unrelated standard on greenhouse gases. Card: publication date 30.09.2004, 17 pages, KT 235 Food Analysis, ICS 67.050, “Replaces PN-EN 14083:2003 – English version”. In the iTeh catalogue (read 03.10.2026) EN 14083:2003 has the status “Published”, stage 90.93 (decision to confirm after review enquiry), with the review from 17.09.2024.

HOW MANY LABORATORIES AND IN WHAT FORM (copy of the accreditation scope database, load up to 17.09.2026, read 03.10.2026). The number 14083 (without ISO) appears in 7 records at 2 laboratories: AB 438 (5), AB 538 (2). In the current PCA documents (read 03.10.2026; AB 538 issue No. 34 of 10.06.2026, AB 438 issue No. 27 of 01.10.2026) the number appears at the same 2 laboratories in 4 reference document cells (2 each), some of which cover several items — hence 7 records; in each document the number of page markers equals the number of PDF pages, without repetitions; a search of all PCA documents downloaded from the BIP on 03.10.2026 found no laboratories outside the database copy. Form “PN-EN 14083:2004” at both. None of these items is suspended; AB 438 has since 01.10.2026 a suspension at its request for the part of the scope marked in bold italics — the items with PN-EN 14083 are not so marked. The “Laboratories” tab (term “PN-EN 14083”) 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). All items: lead and cadmium, ETAAS. AB 438: alcoholic beverages and spirits, fruit, vegetables and their products and vegetable-meat products, mushrooms, cereals and cereal products, milk and milk products, oilseeds — lead (0,010–3,0) mg/kg, cadmium (0,003–2,25) mg/kg; coffee and tea, cocoa, fruit and herbal teas — lead (0,020–6,0), cadmium (0,006–4,5) mg/kg; food supplements — (0,025–6,0) mg/kg; fat emulsions, margarines, fats, meat and meat products, honey, nuts, fish and seafood, confectionery including chocolate, herbs and spices — lead (0,010–6,00) mg/kg and cadmium (0,003–4,50) mg/kg (cadmium also in ready meals). AB 538: food additives, food supplements, coffee and tea, food concentrates, meat, poultry, milk, fruit and vegetables and their products, fish, confectionery, raw herbal materials and products, spices, foods for particular nutritional uses, cereals, frozen food, ready meals, mushrooms, salt, honey, nuts and oilseeds — lead (0,01–20,0) mg/kg, cadmium (0,002–20,0) mg/kg. No laboratory in PCA has chromium or molybdenum according to this standard.

ALONGSIDE THIS STANDARD. The knowledge base already contains PN-EN 13805 — the pressure digestion with which this method begins.

WHERE AN APPARENTLY CORRECT RESULT IS EASY TO GET. With sample preparation: the method assumes a solution after pressure digestion according to EN 13805 (3, 6.1) — another digestion method is already a different procedure; the acidity of calibration and zero member solutions must match the test solution (4.5, 4.6). With the choice of calibration: the calibration method may be used only when its slope does not differ significantly from the slope with standard addition (6.2.2.1) — without this comparison the matrix effect on the result remains unchecked, and the PCA items cover matrices as different as spices, cocoa, food supplements and salt. With the linear range: it is determined and regularly checked, solutions above it are diluted (6.2.2.2). With quality control: reference materials go through all steps from digestion (6.3) — checking a standard alone does not control the digestion. With the scope of the standard: foodstuffs for which vertical standards exist are excluded from it (1). With the result: content in mg/kg of the sample mass as weighed (7) — with dried or concentrated samples it must be known to which mass the result refers.

WHAT WE DO NOT GIVE. We do not quote the required quantifiable concentrations (Table 2), precision data, results of the interlaboratory test or the content of the test report — they lie outside the sample. We have not read EN 13804. We do not give maximum levels of lead and cadmium in food.

Method principle

A food sample is pressure-digested with acid according to EN 13805, and in the resulting solution lead, cadmium, chromium and molybdenum are determined by graphite furnace atomic absorption spectrometry: a drop of solution (e.g. 20 µl) is dried, pyrolysed and atomized in a graphite tube with a matrix modifier, and the absorbance is measured at the element line with background correction. The concentration is read from the calibration function or by standard addition and converted to mg/kg of sample mass.

Applications

• Lead, cadmium, chromium and molybdenum in foodstuffs, except those covered by vertical standards (1)
• Lead and cadmium in food and food supplements — 7 items in the accreditation scopes of 2 laboratories in PCA

Key parameters

Standard

Standard number

PN-EN 14083:2004

Title (PL)

Artykuły żywnościowe — Oznaczanie pierwiastków śladowych — Oznaczanie zawartości ołowiu, kadmu, chromu i molibdenu metodą atomowej spektrometrii absorpcyjnej z atomizacją w piecu grafitowym (GFAAS) po mineralizacji ciśnieniowej

Title (EN)

Foodstuffs — Determination of trace elements — Determination of lead, cadmium, chromium and molybdenum by graphite furnace atomic absorption spectrometry (GFAAS) after pressure digestion

Step-by-step procedure

1. Digestion

   Pressure digestion according to EN 13805, equipment prepared according to EN 13804 (5.1, 6.1). PN-EN 14083:2004 without a withdrawal note in PKN (03.10.2026).

2. Furnace programme

   Optimization of decomposition and atomization temperatures and times, modifier and volume, preferably with the matrix (6.2.1).

3. Calibration

   Zero on the zero member solution, function in the linear range; comparison of slope with standard addition (6.2.2).

4. Measurement

   Absorbance of the test solution (peak area with a platform); dilution outside the range; blanks and reference materials (6.2.2, 6.3).

5. Calculation

   w = a · V · F / m in mg/kg, with blank subtracted (7).

Required equipment and apparatus

Reagents, media and consumables

Health and safety (OHS)

• The standard does not address all safety problems (3, warning)
• Standard solutions of lead, cadmium and potassium chromate are toxic; concentrated acids are corrosive (4.2–4.4)

Frequently asked questions