Foodstuffs - Determination of elements and their chemical species -Determination of Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U and Zn in foodstuffs by inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion

This document specifies a method for the determination of Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U and Zn in foodstuffs by ICP-MS after pressure digestion.
The following foodstuffs were analysed for the elements listed in Table 1 in an interlaboratory study: Banana (deep-frozen), Cocoa powder, Wheat noodle powder, Currant nectar (deep-frozen), Milk powder, Oyster (dried), Celery (dried), Dogfish liver (dried), Liver (deep-frozen), Kale (dried).
Table 1 - Rangea
....

Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U und Zn mit induktiv gekoppelter Plasma-Massenspektrometrie (ICP-MS) nach Druckaufschluss

In diesem Dokument wird ein Verfahren zur Bestimmung von Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U und Zn in Lebensmitteln durch Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) nach Druckaufschluss angegeben.
In einem Ringversuch wurden folgende Lebensmittel auf die in Tabelle 1 aufgeführten Elemente untersucht: Banane (tiefgefroren), Kakaopulver, Weizennudelpulver, Johannisbeernektar (tiefgefroren), Milchpulver, Auster (getrocknet), Sellerie (getrocknet), Katzenhaileber (getrocknet), Leber (tiefgefroren), Grünkohl (getrocknet).
Tabelle 1 - Anwendungsbereich
...

Produits alimentaires - Détermination des éléments et de leurs espèces chimiques - Détermination des éléments Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U et Zn dans les produits alimentaires par spectrométrie de masse avec plasma à couplage inductif (ICP-MS) après digestion sous pression

Le présent document spécifie une méthode de dosage des éléments Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U et Zn dans les produits alimentaires par ICP-MS après digestion sous pression.
Les produits alimentaires suivants ont été analysés par rapport aux éléments répertoriés dans le Tableau 1 lors d’une étude interlaboratoires : banane (surgelée), cacao en poudre, nouille de blé en poudre, nectar de groseille (surgelé), lait en poudre, huître (déshydratée), céleri (déshydraté), foie de saumonette (déshydraté), foie (surgelé), chou vert (déshydraté).
Tableau 1 - Gamme
...

Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U in Zn v živilih z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) po razklopu pod tlakom

Ta dokument določa metodo za določevanje Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U in Zn v živilih z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) po razklopu pod tlakom.
V medlaboratorijski študiji so bila za elemente, navedene v preglednici 1, analizirana naslednja živila:
banana (globoko zamrznjena), kakav v prahu, pšenični rezanci v prahu, ribezov nektar (globoko zamrznjen), mleko v prahu,
ostriga (posušena), zelena (posušena), ribja jetra (posušena), jetra (globoko zamrznjena), ohrovt (posušen).

General Information

Status
Published
Publication Date
11-Jul-2023
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
12-Jul-2023
Due Date
27-Mar-2024
Completion Date
12-Jul-2023

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SLOVENSKI STANDARD
01-oktober-2023
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje Ag, As,
Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U in Zn v živilih z masno spektrometrijo z
induktivno sklopljeno plazmo (ICP-MS) po razklopu pod tlakom
Foodstuffs - Determination of elements and their chemical species - Determination of Ag,
As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U and Zn in foodstuffs by inductively coupled
plasma mass spectrometry (ICP-MS) after pressure digestion
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U und Zn mit induktiv gekoppelter
Plasma-Massenspektrometrie (ICP-MS) nach Druckaufschluss
Produits alimentaires - Détermination des éléments et de leurs espèces chimiques -
Détermination des éléments Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U et Zn dans
les produits alimentaires par spectrométrie de masse avec plasma à couplage inductif
(ICP-MS) après digestion sous pression
Ta slovenski standard je istoveten z: EN 17851:2023
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17851
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2023
EUROPÄISCHE NORM
ICS 67.050
English Version
Foodstuffs - Determination of elements and their chemical
species -Determination of Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni,
Pb, Se, Tl, U and Zn in foodstuffs by inductively coupled
plasma mass spectrometry (ICP-MS) after pressure
digestion
Produits alimentaires - Détermination des éléments et Lebensmittel - Bestimmung von Elementen und ihren
de leurs espèces chimiques - Détermination des Verbindungen - Bestimmung von Ag, As, Cd, Co, Cr, Cu,
éléments Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl, U Mn, Mo, Ni, Pb, Se, Tl, U und Zn mit induktiv
et Zn dans les produits alimentaires par spectrométrie gekoppelter Plasma-Massenspektrometrie (ICP-MS)
de masse avec plasma à couplage inductif (ICP-MS) nach Druckaufschluss
après digestion sous pression
This European Standard was approved by CEN on 5 June 2023.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17851:2023 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Reagents . 5
6 Apparatus . 8
6.1 General . 8
6.2 ICP-MS. 8
7 Sampling . 8
8 Procedure. 8
8.1 Digestion . 8
8.2 Inductively coupled plasma mass spectrometry (ICP-MS). 9
8.2.1 ICP-MS working conditions . 9
8.2.2 Determination by ICP-MS . 9
8.3 Quality control of the analysis .10
9 Evaluation .11
9.1 Calculation of element contents in foodstuffs.11
9.2 Limits of quantification .11
9.3 Reliability of the procedure .12
10 Precision .12
10.1 General .12
10.2 Repeatability .12
10.3 Reproducibility .13
11 Test report .18
12 Explanations and notes .18
Annex A (normative) Potential spectral interferences of recommended Isotopes .19
Annex B (informative) Precision Data .23
Annex C (informative) Trueness of the procedure.38
Bibliography .39

European foreword
This document (EN 17851:2023) 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 January 2024, and conflicting national standards shall
be withdrawn at the latest by January 2024.
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.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the United
Kingdom.
1 Scope
This document specifies a procedure for the determination of Ag, As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Tl,
U and Zn in foodstuffs by inductively coupled plasma mass spectrometry (ICP-MS) after pressure
digestion.
The following foodstuffs were analysed for the elements listed in Table 1 in an interlaboratory study:
Banana (deep-frozen), Cocoa powder, Wheat noodle powder, Currant nectar (deep-frozen), Milk powder,
Oyster (dried), Celery (dried), Dogfish liver (dried), Liver (deep-frozen), Kale (dried).
a
Table 1 — Validated range
Mass fraction
mg/kg
Element
Lower range Upper range
Arsenic 0,02 36,6
Lead 0,004 0,58
Cadmium 0,006 15,2
Chromium 0,06 5,71
Cobalt 0,03 7,49
Copper 0,71 74,0
Manganese 0,31 73,5
Molybdenum 0,05 1,88
Nickel 0,11 11,0
Selenium 0,06 8,70
Silver 0,011 1,98
Thallium 0,008 0,12
Uranium 0,003 0,26
Zinc 1,8 1 582
a
Table 1 lists the ranges analysed in the interlaboratory study, indicating for each element the lowest and
highest content found in the ten analysed food matrices (see Annex B, Table B.1 to Table B.14).
The lower limit of the procedure’s range varies depending on the food matrix and the food’s water content.
It is a laboratory-specific value and is specified by the laboratory for each element when calculating the limit
of quantification (see 9.2).
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. 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
EN 15765, Foodstuffs - Determination of trace elements - Determination of tin by inductively coupled
plasma mass spectrometry (ICP-MS) after pressure digestion
EN 17264, Foodstuffs - Determination of elements and their chemical species - Determination of aluminium
by inductively coupled plasma mass spectrometry (ICP-MS)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
The sample is digested. For the digestion the pressure digestion process in EN 13805 shall be used, in the
case of foodstuffs with a low water content, after adding water. In the digestion solution, the elements
silver, arsenic, cadmium, cobalt, chromium, copper, manganese, molybdenum, nickel, lead, selenium,
thallium, uranium and zinc are quantified by ICP-MS. For this purpose, the digestion solution is nebulized
and the aerosol is transferred to an inductively coupled argon plasma where the elements are ionized.
The ions are transferred via a system of cones into a mass spectrometer, where they are separated
according to mass-to-charge ratio and detected by pulse and/or analogue detector.
The respective content of the elements mentioned in Clause 1 is understood as the total content
measured using this described procedure. It is expressed in mg/kg or mg/l, depending on the sample
type.
For other elements not specified within the scope, other documents can be considered, e.g. EN 15763. For
the determination of aluminium and tin in foodstuffs refer to EN 17264 and EN 15765.
5 Reagents
The chemicals, gases and water used shall be free enough from the elements to be determined to not
affect the results. Unless otherwise specified, “solutions” are understood to be aqueous solutions.
5.1 Nitric acid, mass fraction of min. ω = 65 %, density ρ ≈ 1,4 g/ml.
5.2 Stock solutions
A commercially available multi-element stock solution, for example with ρ = 10 mg/l, can be used for
silver, cadmium, cobalt, chromium, copper, manganese, molybdenum, nickel, lead, thallium, uranium and
for example with ρ = 100 mg/l for arsenic, selenium and zinc.
Alternatively, commercially available single-element stock solutions, for example with ρ = 1 000 mg/l,
can be used.
When using single-element stock solutions, attention shall be paid that they are suitable for ICP-MS, i.e.
are of sufficiently high purity, to generate no additional contamination with other elements to be
determined. If mixing the single-element stock solutions, attention shall also be paid to chemical
compatibility.
NOTE Depending on the manufacturer, stock solutions with 10 000 mg/l can also be used i
...

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