SIST EN 16943:2017
(Main)Foodstuffs - Determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc by ICP-OES
Foodstuffs - Determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc by ICP-OES
This European Standard describes a method for the determination of minerals and trace elements in foodstuffs using optical emission spectrometry with inductively coupled plasma (ICP-OES) after pressure digestion.
This method has been validated in an interlaboratory study according to ISO 5725 [1] on children's food soya, cheese, chicken meat, wheat flour, apple juice, lobster and milk, with calcium ranging from 70 mg/kg to 7178 mg/kg, with copper ranging from 0,60 mg/kg to 16,40 mg/kg, with iron ranging from 0,88 mg/kg to 77 mg/kg, with potassium ranging from 605 mg/kg to 14 312 mg/kg, with magnesium ranging from 45 mg/kg to 1 174 mg/kg, with manganese ranging from 0,44 mg/kg to 5,12 mg/kg, with sodium ranging from 11 mg/kg to 2 220 mg/kg, with phosphorus ranging from 72 mg/kg to 9 708 mg/kg, with sulfur ranging from 26 mg/kg to 8 542 mg/kg and with zinc ranging from 0,16 mg/kg to 43,5 mg/kg.
Lebensmittel - Bestimmung von Calcium, Kupfer, Eisen, Magnesium, Mangan, Phosphor, Kalium, Natrium, Schwefel und Zink mit ICP OES
Diese Europäische Norm beschreibt ein Verfahren zur Bestimmung von Mineralstoffen und Spurenelementen in Lebens¬mitteln mit der optischen Emissionsspektrometrie mit induktiv gekoppeltem Plasma (en: optical emission spectrometry with inductively coupled plasma, ICP-OES) nach Druckaufschluss.
Dieses Verfahren wurde in einem Ringversuch nach ISO 5725 [1] unter Verwendung von Kindernahrung auf Sojabasis, Käse, Hühnchenfleisch, Weizenmehl, Apfelsaft, Hummer und Milch, mit Calcium im Bereich von 70 mg/kg bis 7 178 mg/kg, mit Kupfer im Bereich von 0,60 mg/kg bis 16,40 mg/kg, mit Eisen im Bereich von 0,88 mg/kg bis 77 mg/kg, mit Kalium im Bereich von 605 mg/kg bis 14 312 mg/kg, mit Magnesium im Bereich von 45 mg/kg bis 1 174 mg/kg, mit Mangan im Bereich von 0,44 mg/kg bis 5,12 mg/kg, mit Natrium im Bereich von 11 mg/kg bis 2 220 mg/kg, mit Phosphor im Bereich von 72 mg/kg bis 9 708 mg/kg, mit Schwefel im Bereich von 26 mg/kg bis 8 542 mg/kg und mit Zink im Bereich von 0,16 mg/kg bis 43,5 mg/kg validiert.
Produits alimentaires - Dosage du calcium, du cuivre, du fer, du magnésium, du manganèse, du phosphore, du potassium, du sodium, du soufre et du zinc par ICP-OES
La présente Norme européenne décrit une méthode de dosage des minéraux et des éléments traces dans les produits alimentaires par spectrométrie d’émission optique à plasma induit par haute fréquence (ICP-OES) après digestion sous pression.
Cette méthode a été validée lors d’une étude interlaboratoires réalisée conformément à l’ISO 5725 [1] sur des aliments pour enfants à base de soja, du fromage, de la viande de poulet, de la farine de blé, du jus de pomme, du homard et du lait ayant une teneur en calcium comprise entre 70 mg/kg et 7178 mg/kg, une teneur en cuivre comprise entre 0,60 mg/kg et 16,40 mg/kg, une teneur en fer comprise entre 0,88 mg/kg et 77 mg/kg, une teneur en potassium comprise entre 605 mg/kg et 14 312 mg/kg, une teneur en magnésium comprise entre 45 mg/kg et 1 174 mg/kg, une teneur en manganèse comprise entre 0,44 mg/kg et 5,12 mg/kg, une teneur en sodium comprise entre 11 mg/kg et 2 220 mg/kg, une teneur en phosphore comprise entre 72 mg/kg et 9 708 mg/kg, une teneur en soufre comprise entre 26 mg/kg et 8 542 mg/kg et une teneur en zinc comprise entre 0,16 mg/kg et 43,5 mg/kg.
Živila - Določevanje kalcija, bakra, železa, magnezija, mangana, fosforja, kalija, natrija, žvepla in cinka z ICP-OES
Ta evropski standard opisuje metodo za določanje mineralov in elementov v sledovih v živilih z uporabo optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP-OES) po razklopu pod tlakom.
Ta metoda je bila potrjena v medlaboratorijski študiji v skladu s standardom ISO 5725 [1] o otroški hrani, soji, siru, piščančjem mesu, pšenični moki, jabolčnem soku, jastogu in mleku s kalcijem v razponu 70–7178 mg/kg, z bakrom v razponu 0,60–16,40 mg/kg, z železom v razponu 0,88–77 mg/kg, s kalijem v razponu 605–14.312 mg/kg, z magnezijem v razponu 45–1174 mg/kg, z manganom v razponu 0,44–5,12 mg/kg, z natrijem v razponu 11–2220 mg/kg, s fosforjem v razponu 72–9708 mg/kg, z žveplom v razponu 26–8542 mg/kg in s cinkom v razponu 0,16–43,5 mg/kg.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Calcium, Kupfer, Eisen, Magnesium, Mangan, Phosphor, Kalium, Natrium, Schwefel und Zink mit ICP OESProduits alimentaires - Dosage du calcium, du cuivre, du fer, du magnésium, du manganèse, du phosphore, du potassium, du sodium, du soufre et du zinc par ICP-OESFoodstuffs - Determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc by ICP-OES67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 16943:2017SIST EN 16943:2017en,fr,de01-julij-2017SIST EN 16943:2017SLOVENSKI
STANDARD
SIST EN 16943:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16943
May
t r s y ICS
x yä r w r English Version
Foodstuffs æ Determination of calciumá copperá ironá magnesiumá manganeseá phosphorusá potassiumá sodiumá sulfur and zinc by ICPæOES Produits alimentaires æ Dosage du calciumá du cuivreá du ferá du magnésiumá du manganèseá du phosphoreá du potassiumá du sodiumá du soufre et du zinc par ICPæOES
Lebensmittel æ Bestimmung von Calciumá Kupferá Eisená Magnesiumá Manganá Phosphorá Kaliumá Natriumá Schwefel und Zink mit ICP OES This European Standard was approved by CEN on
t r February
t r s yä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
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CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x { v uã t r s y ESIST EN 16943:2017
EN 16943:2017 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Reagents . 5 5 Apparatus . 7 6 Procedure. 8 6.1 Sample preparation . 8 6.2 Optical emission spectrometry with inductively coupled plasma . 8 6.2.1 ICP-OES working conditions . 8 6.2.2 Determination with ICP-OES . 8 6.3 Quality control of the analysis . 10 7 Calculation . 10 8 Precision . 11 8.1 General . 11 8.2 Repeatability . 11 8.3 Reproducibility . 11 9 Test report . 14 Annex A (informative)
Spectral interferences . 15 Annex B (informative)
Precision Data . 18 B.1 Details on the inter-laboratory study . 18 Bibliography . 30
SIST EN 16943:2017
EN 16943:2017 (E) 3 European foreword This document (EN 16943:2017) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2017, and conflicting national standards shall be withdrawn at the latest by November 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16943:2017
EN 16943:2017 (E) 4 1 Scope This European Standard describes a method for the determination of calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc in different foodstuffs using optical emission spectrometry with inductively coupled plasma (ICP-OES) after pressure digestion. This method has been validated in an interlaboratory study according to ISO 5725 [1] on infant formula soya based, cheese, chicken meat, wheat flour, apple juice, lobster and milk (see elements ranges Table 1 and validation data in Annex B). HorRat values greater than 2 have been observed for certain analyte/matrix combinations during the validation study. Table 1 — Validated element ranges Element Range mg/kg Calcium 70 to 7178 Copper 0,60 to 16,40 Iron 0,88 to 77 Magnesium 45 to 1 174 Manganese 0,44 to 5,12 Phosphorus 72 to 9 708 Potassium 605 to 14 312 Sodium 11 to 2 220 Sulfur 26 to 8 542 Zinc 0,16 to 43,5 At European or International level, vertical standards for the determination of specific minerals can exist, e.g. for milk and milk products or for animal and vegetable fats and oils [2]. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 13804, Foodstuffs - Determination of elements and their chemical species - General considerations and specific requirements EN 13805, Foodstuffs - Determination of trace elements - Pressure digestion 3 Principle After digestion of the sample with the pressure digestion process described in EN 13805, calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc are determined quantitatively with the ICP-OES [2]. The digestion solution is nebulized, the aerosol is directed into an inductively coupled argon plasma, where the elements are atomized and excited for radiation. The emission radiation is resolved spectrally and its intensity determined at element-specific wavelengths with a detector system. Ionization interference can be minimized using an ionization buffer. SIST EN 16943:2017
EN 16943:2017 (E) 5 4 Reagents The concentration of the elements to be determined shall be low enough in the reagents and water not to affect the results. 4.1 Nitric acid, minimum w = 65 % 1, density about 1,4 g/ml 4.2 Hydrochloric acid, w = 30 %, density = 1,15 g/ml 4.3 Hydrogen peroxide, w = 30 % Hydrogen peroxide (4.3) can contain phosphoric acid as a stabilizing agent. Hydrogen peroxide stabilized with phosphoric acid contaminates the samples with phosphorus and thus leads to incorrect results. 4.4 Caesium chloride solution as ionization buffer, e.g. w = 10 % (see 6.2.2) 4.5 Internal standard, e.g. scandium, ytterbium, yttrium Depending on the matrix, e.g. for samples with high total salt content, the application of an internal standard can be advantageous in order to reduce physical interference. In doing so, it shall be ensured that no faults from line interference result due to the internal standard. NOTE It has been shown that if an internal standard is used, it is applicable to all elements mentioned in the scope. 4.6 Stock solutions,
= 1 000 mg/l 2 per element Calcium, copper, iron, magnesium, manganese, phosphorus, potassium, sodium, sulfur and zinc individual element stock solutions and internal standard used. The individual element stock solutions may not contain any of the elements to be determined here as accompanying substances or impurities, which could affect the correctness of the results. Alternatively, commercial mixed stock solutions can also be used. 4.7 Standard solutions,
= 100 mg/l per element Copper, iron, manganese and zinc standard solution, produced by dilution of the respective stock solution (4.6). Pour 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (4.1) and mix. After cooling to room temperature, add exactly 5 ml respectively of the copper, iron, manganese and zinc stock solution (4.6) by pipette and fill up with water to the mark. These standard solutions are stable for at least six months. 4.8 Element reference solutions 4.8.1 General The concentrations of the reference solutions indicated in 4.8.3 to 4.8.6 serve as examples and shall be modified corresponding to the instrument sensitivity, the direction of viewing (axial or radial) and the concentration range to be examined, if necessary. If possible, the calibration shall be performed in the
1 w = mass fraction 2
SIST EN 16943:2017
EN 16943:2017 (E) 6 linear range. Minimum 3, in the nonlinear range 5, reference solutions of different concentrations should be prepared for the calibration. The concentration of the reagents (acids, if applicable ionization buffer and internal standard) shall correspond to the sample measuring solution. For reasons of stability and purity, the phosphorus and sulfur reference solutions should be prepared separately from the multi-element reference solutions of the cations. 4.8.2 Preparation of the flask Pour 10 ml to 20 ml of water into a 100-ml volumetric flask, add 10 ml of nitric acid (4.1) and 2 ml of hydrochloric acid (4.2) and mix. After cooling to room temperature, add stock (4.6) and standard solutions (4.7) by pipette. If using an ionization buffer, add 10 ml of 10 % caesium chloride solution (4.4). If using an internal standard (4.5), add the corresponding amount. Alternatively, the ionization buffer and/or the internal standard can be pumped via a Y-piece into the sample flow during the measurement.
These reference solutions are stable for a month. The following data under 4.8.3 to 4.8.6 serve as examples and shall be adapted corresponding to the device sensitivity and the emission wavelength selected, and the direction of viewing (axial or radial), if necessary. 4.8.3 Reference solution 1 Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2): — 2,0 ml calcium \3)
= 20 mg/l calcium; — 1,0 ml magnesium \
= 10 mg/l magnesium; — 2,0 ml potassium \
= 20 mg/l potassium; — 1,0 ml sodium \
= 10 mg/l sodium; Furthermore, pipette the following amounts of standard solutions (4.7) into the same flask and fill up to the mark with water: — 0,50 ml copper \
= 0,5 mg/l copper; — 0,50 ml iron \
= 0,5 mg/l iron; — 0,50 ml manganese \
= 0,5 mg/l manganese; — 0,50 ml zinc \
= 0,5 mg/l zinc. 4.8.4 Reference solution 2 Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2): — 10,0 ml calcium \
= 100 mg/l calcium; — 5,0 ml magnesium \
= 50 mg/l magnesium; — 10,0 ml potassium \
= 100 mg/l potassium; — 5,0 ml sodium \
= 50 mg/l sodium.
3) the sign "\ 6 means: "which leads to a mass concentration of" SIST EN 16943:2017
EN 16943:2017 (E) 7 Furthermore, pipette the following amounts of standard solutions (4.7) into the same flask and fill up to the mark with water: — 2,0 ml copper \
= 2,0 mg/l copper; — 2,0 ml iron \
= 2,0 mg/l iron; — 2,0 ml manganese \
= 2,0 mg/l manganese; — 2,0 ml zinc \
= 2,0 mg/l zinc. 4.8.5 Reference solution 3 Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2): — 20,0 ml calcium \
= 200 mg/l calcium; — 10,0 ml magnesium \
= 100 mg/l magnesium; — 20,0 ml potassium \
= 200 mg/l potassium; — 10,0 ml sodium \
= 100 mg/l sodium. Furthermore, pipette the following amounts of standard solutions (4.7) into the same flask and fill up to the mark with water: — 5,0 ml copper \
= 5,0 mg/l copper; — 5,0 ml iron \
= 5,0 mg/l iron; — 5,0 ml manganese \
= 5,0 mg/l manganese; — 5,0 ml zinc \
= 5,0 mg/l zinc. 4.8.6 Reference solutions phosphorus and sulfur Pipette the following amounts of stock solutions (4.6) into the prepared 100-ml volumetric flask (4.8.2) and fill up to the mark with water: — 1,0 ml respectively phosphorus and sulfur \
= 10,0 mg/l phosphorus and sulfur; — 5,0 ml respectively phosphorus and sulfur \
= 50,0 mg/l phosphorus and sulfur; — 10,0 ml respectively phosphorus and sulfur \
= 100,0 mg/l phosphorus and sulfur. 4.9 Zero value solution The zero value solution contains water, 10 ml of nitric acid (4.1), 2 ml of hydrochloric acid (4.2), if applicable 10 ml caesium chloride solution (4.4) and a corresponding amount of internal standard (4.5) in 100 ml. 5 Apparatus 5.1 General All equipment and labware that come into direct contact with the sample and the solutions used shall be carefully pretreated/cleaned corresponding to EN 13804 to minimize the blank value. 5.2 ICP-OES, optical emission spectrometer with inductively coupled argon plasma, sample supply and atomization system as well as device control and evaluation unit. SIST EN 16943:2017
EN 16943:2017 (E) 8 6 Procedure 6.1 Sample preparation Mineralize the sample in a pressure digestion corresponding to EN 13805. In the case of dry, powdery or free-flowing materials (water content below 20 %), add 2 ml of water in relation to a test portion of 400 mg, and mix intensively so that the sample is well suspended in the water. Add nitric acid (4.1) and mix. For the determination of iron in order to avoid adsorption losses, add 0,5 ml to 1 ml of hydrochloric acid (4.2) to the digestion vessel, in addition to the nitric acid (4.1). The amount of hydrochloric acid depends on the amount of nitric acid used. Do not add the hydrochloric acid before/until the termination/expiration of the spontaneous reaction caused by the nitric acid. Seal the digestion vessel immediately after addition of the hydrochloric acid. The pressure digestion should be started shortly afterwards. Use digestion conditions according to the device manufacturer, the reactivity of the sample, the maximum pressure stability of the digestion vessel and the attainable temperature. NOTE The trueness of the determination of the other elements is not impaired by the addition of hydrochloric acid during the digestion. Fill up the digestion solution obtained according to EN 13805 after the pressure digestion to a definite volume, e.g. 20 ml. It can be used directly or after dilution for the following element determinations. The same concentration of acids, if applicable internal standard and ionization buffer, shall be present in all measuring solutions as in the reference solutions. 6.2 Optical emission spectrometry with inductively coupled plasma 6.2.1 ICP-OES working conditions Ensure that the device is set corresponding to the manufacturer's data and the plasma is ignited. After sufficient heating and stabilization of the device, optimize the settings [3], [4]. 6.2.2 Determination with ICP-OES Start the measurements after optimizing the device. The following wavelengths (Table 2), which have been tested for possible interference (see Table A.1), are recommended for determination of elements and for internal standards (Table 3). The wavelength data in the device-specific spectral libraries can deviate. Further wavelengths can be used, although these shall be tested for potential interference in individual cases. SIST EN 16943:2017
EN 16943:2017 (E) 9 Table 2 — Recommended wavelengths for element determination Element Wavelengths nm Possible interference Calcium 317,93 315,89 422,67 Ce, Fe, Mo, V Co, Mo, OH band Mo, V, Zr Copper 324,75 327,40 Cr, Fe, Mo, Nb, Ti, U Co, Nb, Ti, U Iron 259,94 238,20 Co, Mn, Nb Co Magnesium 279,08 285,21 Fe, Nb, Rh Cr, Fe, Mo, W Manganese 257,61 293,31 Cr, Fe, Mo, W Al, Cr, Fe, Ti Phosphorus 213,62 214,91 177,43 Co, Cu, Fe, Mo, Zn Al, Cu, Fe, Mg Cu Potassium 766,49 769,90 404,72 Ar, Ba, Mg, Ba Ba Sodium 589,59 330,24 Ar, Ba, V Zn Sulfur 181,97 180,67 182,56 B, Nb, Ni, Pb As, Ca, Co, Ni, Si B, Cu, Mg Zinc 213,86 206,20 Al, As, Cu, Fe, Mg, Ni Cr, Nb Table 3 — Recommended wavelengths for internal standards Element Wavelength nm Scandium 361,38 Ytterbium 328,94 Yttrium 371,03 SIST EN 16943:2017
EN 16943:2017 (E) 10 When determining sodium and potassium, ionization interferences are generally present. In general, an ionization buffer, e.g. caesium chloride (w = 1 % in the measurement solution), should be used for the axial recording of the plasma emission. In the case of radial recording of the emission intensity, the user of this standard shall establish whether the use of an ionization buffer can be omitted by optimizing the observation height and the gas settings. If element lines below 190 nm are applied, ensure sufficient inert gas purging between the plasma and inlet gap as well as the spectrometer so that oxygen absorption cannot cause any drifting of intensities. If the ionization buffer is added via a Y-piece, adjust volume ratios so that the solution that enters the atomizer or plasma contains an excess of caesium chloride. Measure zero value solution (4.9) and reference solutions (4.8) and prepare a calibration curve using emission intensities or peak areas and concentrations. In the case of complex matrices, the standard addition method may be necessary. Aspirate sample solution and measure it. The determined peak areas or intensities are converted via calibration curve using linear regression into concentration units. Ensure sufficient time for rinsing before the next measurement in case of samples with high element concentrations. Rinse performance can be monitored with zero value solution (4.9). When making dilutions, ensure that the diluted measuring solutions have the same concentrations of reagents as the original measuring solutions. 6.3 Quality control of the analysis For quality control, analyse control samples with reliably known contents of the elements to be determined in parallel to every measurement series. The control samples should pass through all analytical steps, beginning with the digestion. Likewise, prepare reagent blank solutions and measure for every digestion series, taking into account all process steps. To check for matrix effect spiking experiments should be performed by adding a known concentration of the elements to the measurement solution. 7 Calculation Calculate the mass fraction w in milligrams per kilogram or litre of sample according to Formula (1): aVFwm⋅⋅==(1)=where=a is the mass fraction of the element in the sample solution in milligrams per litre; V is the volume of the sample solution after digestion in millilitres; F is the dilution factor of the sample measuring solution; m is the mass of the test portion in grams or the sample volume in millilitres used for digestion. Causes of increased element contents in the blank value solution shall be clarified and, if necessary, deducted from the calculation of the results. SIST EN 16943:2017
EN 16943:2017 (E) 11 8 Precision 8.1 General Details of the inter-laboratory test of the precision of the methods are summarized in Annex B. The values derived from this test may not be applicable to analyte concentration ranges and matrices other than given in Annex B. 8.2 Repeatability The absolute difference between two independent single test results obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short time interval, will in no more than 5 % of the cases exceed the values of r given in Table 4. 8.3 Reproducibility The absolute difference between two single test results obtained using the same method on identical test material in different laboratories by different operators using the equivalent equipment will in no more than 5 % of the cases exceed the values of R given in Table 4. Table 4 — Precision data Sample/elements x mg/kg r mg/kg R mg/kg Infant formula (soya based) Calcium 6 191 591 1 381 Copper 4,51 0,54 1,40 Iron 77,0 5,9 15,0 Magnesium 599 72 128 Manganese 2,19 0,29 0,84 Phosphorus 4 129 399 909 Potassium 6 733 769 1 035 Sodium 2 220 228 304 Sulfur 1 234 133 370 Zinc 43,5 3,2 8,4 Cheese Calcium 7 178 394 930 Copper 14,66 0,96 2,53 Iron 2,3 0,4 1,1 Magnesium 587 58 104 Manganese 0,2 - - Phosphorus 9 708 1 080 782 Potassium 8 397 879 1 293 Sodium 2 039 132 235 SIST EN 16943:2017
EN 16943:2017 (E) 12 Sample/elements x mg/kg r mg/kg R mg/kg Sulfur 5 764 504 1 176 Zinc 38,4 3,5 7,1 Chicken meat Calcium 186 18 33 Coppera 1,50 0,70 1,35 Iron 24,0 4,4 7,7 Magnesium 1 147 116 242 Manganese 1,35 0,17 0,46 Phosphorus 9 034 1 022 1 911 Potassium 14 312 473 2 459 Sodium 1 303 124 145 Sulfur 8 542 465 1 464 Zinc 24,8 3,0 4,6 Wheat flour Calcium 305 23 34 Copper 2,51 0,33 0,90 Iron 15,3 1,9 3,9 Magnesium 397 27 74 Manganese 5,12 0,40 0,92 Phosphorus 1 466 119 258 Potassium 1 325 163 203 Sodiuma 11 3 8 Sulfur 1 694 149 320 Zinc 11,2 1,2 1,5 Apple juice Calcium 70 6 9 Copper 0,04 - - Iron 0,88 0,11 0,19 Magnesium 45 3 10 Manganese 0,44 0,05 0,09 Phosphorus 72 7 15 Potassium 1 090 99 196 SIST EN 16943:2017
EN 16943:2017 (E) 13 Sample/elements x mg/kg r mg/kg R mg/kg Sodium 19 4 9 Sulfur 26 6 13 Zinc 0,16 0,04 0,09 Lobster Calcium 183 25 32 Copper 16,40 2,63 3,13 Iron 12,1 2,2 2,9 Magnesium 85 9 20 Manganese 1,20 0,16 0,27 Phosphorus 973 86 194 Potassium 871 88 153 Sodium 1 175 9 217 Sulfur 876 77 185 Zinc 13,9 1,8 3,1 Milk Calcium a 516 45 209 Copper 0,60 0,12 0,21 Iron 7,7 0,7 1,4 Magnesium 53 4 11 Manganese 0,04 - - Phosphorus a 319 30 130 Potassium 605 85 148 Sodium 186 14 34 Sulfur 177 13 44 Zinc 5,1 0,4 0,9 a This element/matrix combination lead to a Horrat value of greater than 2 in the validation study, see Annex B. SIST EN 16943:2017
EN 16943:2017 (E) 14 9 Test report The test report should comply with EN ISO/IEC 17025 [5] and shall contain at least the following data: a) all information necessary for the complete identification of the sample; b) the test method used and the elements to be determined with reference to this European standard; c) the results obtained and the units in which they are specified; d) the date of the sampling procedure (if known); e) the date when the analyses was finished; f) all operating details not specified in this European Standard or regarded as optional, together with details of any incidents occurred when performing the method which might have influenced the test results. SIST EN 16943:2017
EN 16943:2017 (E) 15 Annex A (informative)
Spectral interferences The line interferences were checked with three device systems of different design and resolution capacity (Perkin Elmer Optima 3000, Spectro Ciros, Varian Vista). The interferences listed in the following Table A.1 have been checked with the concentrations indicated. Line interference is generally affected by the resolution of the spectrometer used and the background correction and shall therefore always be checked on the spectrometer used for the measurement. Table A.1 can thus only serve as a starting point for the level of an interference. Table A.1 — Line interferences Element (Analyte) Wavelength
nm Interfering element Concentration of interfering element mg/l Apparent analyte concentration mg/l Calcium 317,93 Ce Fe Mo V 10 50 10 10 > 0,01 < 0,01 < 0,01 > 0,01 315,89 Co Mo 10 10 > 0,01 > 0,01 422,67 Mo V Zr 10 10 10 < 0,01 > 0,01 < 0,01 Copper 324,75 Cr Fe Mo Nb Ti U 10 50 10 10 10 10 < 0,01 < 0,01 < 0,01 > 0,1 < 0,01 < 0,01 327,40 Co Nb Ti U 10 10 10 10 < 0,01 > 0,01 < 0,01 > 0,01 Iron 259,94 Co Mn Nb 10 10 10 < 0,01 < 0,01 < 0,01 238,20 Co 10 < 0,01 SIST EN 16943:2017
EN 16943:2017 (E) 16 Element (Analyte) Wavelength
nm Interfering element Concentration of interfering element mg/l Apparent analyte concentration mg/l Magnesium 279,08 Fe Nb Rh 50 10 10 > 0,01 > 0,1 > 0,1 285,21 Cr Fe Mo W 10 50 10 10 < 0,01 < 0,01 < 0,01 < 0,01 Manganese 257,61 Cr Fe Mo W 10 50 10 10 < 0,01 < 0,01 < 0,01 < 0,01 293,31 Al Cr Fe Ti 50 10 50 10 < 0,01 < 0,01 < 0,01 < 0,01 Phosphorus 213,62 Co Cu Fe Mo Zn 10 10 50 10 50 < 0,01 > 0,2 < 0,01 > 0,01 > 0,01 214,91 Al Cu Fe Mg 50 10 50 200 < 0,01 > 0,05 > 0,05 < 0,01 177,43 Cu 10 > 0,01 Potassium 766,49 Ba Mg 10 200 < 0,01 < 0,01 769,90 Ba 10 < 0,01 404,72 Ba 10 < 0,01 Sodium 589,59 Ba V 10 10 > 1 < 0,01 330,24 Zn 10 > 5 SIST EN 16943:2017
EN 16943:2017 (E) 17 Element (Analyte) Wavelength
nm Interfering element Concentration of interfering element mg/l Apparent analyte concentration mg/l Sulfur 181,97 B Nb Ni Pb 10 10 10 10 < 0,1 < 0,1 < 0,1 < 0,1 180,67 As Ca Co Ni Si 10 200 10 10 50 < 0,1 > 2 < 0,1 < 0,1 < 0,1 182,56 B Cu Mg 10 10 200 > 1 < 0,1 < 0,1 Zinc 213,86 Al As Cu Fe Mg Ni 50 10 10 50 200 10 < 0,01 < 0,01 > 0,01 > 0,01 < 0,01 > 0,05 206,20 Cr Nb 10 10 > 0,2 < 0,01 SIST EN 16943:2017
EN 16943:2017 (E) 18 Annex B (informative)
Precision Data B.1 Details on the inter-laboratory study The data given in Table B.1 to Table B.10 were obtained in an inter-laboratory study [2] organized in 2011 by the Working Group “Elementanalytik” of the Federal Office for Consumer Protection and Food Safety (Bundesamt für Verbraucherschutz und Lebensmittelsicherheit — BVL) according to the German Food and Feed Act, Paragraph 64 (Lebensmittel- und Futtermittelgesetzbuch-LFGB, § 64) in accordance with ISO 5725-2á
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s u participating laboratoriesä Each quantitative value of a laboratory results from a double determination or, in the case of cheese (double blind), from a fourfold determination. The materials used in the interlaboratory study have been fresh materials (milk, apple juice and lobster) and dry materials (wheat flour, infant formula, cheese and chicken meat). Four materials were reference materials (NCS ZC73009 wheat, NCS ZC73016 chicken, NRC LUTS-1 non defatted lobster hepatopancreas (approximately 8 % fat) and dried low fat fresh cheese (approximately 4,5 % fat, 23 % carbohydrates and 67 % protein) as a former proficiency test material). The infant formula soya based material contained 58 % carbohydrates, 24 % fat and 13 % protein. The apple juice was a commercial available product mainly containing 10 % carbohydrates. The milk with a typical fat content of 4 %, 2,5 % protein, a dry weight of 12 % and a carbohydrate content of 8,5 % was enriched with minerals and proteins. For calcium and phosphorous the reproducibility was relatively high. The laboratories did not use the same procedure for homogenization which led to insufficiently homogenous partition of the casein fraction in the sample during sample preparation. In Table B.11 the data concerning trueness determined by the use of reference material is given. SIST EN 16943:2017
EN 16943:2017 (E) 19 Table B.1 — Validation data for calcium Statistical parameter Calcium Infant fo
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