SIST EN 17264:2019

SLOVENSKI STANDARD
SIST EN 17264:2019
01-november-2019
Živila - Določevanje elementov in njihovih spojin - Določevanje aluminija z masno
spektrometrijo z induktivno sklopljeno plazmo (ICP-MS)
Foodstuffs - Determination elements and their chemical species - Determination of
aluminium by inductively coupled plasma mass spectrometry (ICP-MS)
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Aluminium mit der Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage de
l'aluminium par spectrométrie de masse avec plasma à couplage inductif (ICP-MS)
Ta slovenski standard je istoveten z: EN 17264:2019
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
SIST EN 17264:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 17264:2019

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SIST EN 17264:2019


EN 17264
EUROPEAN STANDARD

NORME EUROPÉENNE

September 2019
EUROPÄISCHE NORM
ICS 67.050
English Version

Foodstuffs - Determination of elements and their chemical
species - Determination of aluminium by inductively
coupled plasma mass spectrometry (ICP-MS)
Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren
espèces chimiques - Dosage de l'aluminium par Verbindungen - Bestimmung von Aluminium mittels
spectrométrie de masse avec plasma à couplage Massenspektrometrie mit induktiv gekoppeltem
inductif (ICP-MS) Plasma (ICP-MS)
This European Standard was approved by CEN on 28 July 2019.

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, Turkey 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17264:2019 E
worldwide for CEN national Members.

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SIST EN 17264:2019
EN 17264:2019 (E)
Contents Page
European foreword . 3
1 Scope . 3
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 6
7 Procedure. 7
7.1 Digestion . 7
7.2 Mass spectrometry with inductively coupled plasma . 8
8 Evaluation . 10
8.1 Calculation . 10
8.2 Precision . 10
8.3 Repeatability . 10
8.4 Reproducibility . 11
9 Test report . 11
Annex A (informative) Results of interlaboratory study . 12
Annex B (normative) Explanation notes . 14
Bibliography . 16

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SIST EN 17264:2019
EN 17264:2019 (E)
European foreword
This document (EN 17264:2019) 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 March 2020, and conflicting national standards shall
be withdrawn at the latest by March 2020.
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, 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, Turkey and the
United Kingdom.
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EN 17264:2019 (E)
1 Scope
This document specifies a method for the determination of aluminium in food by inductively coupled
plasma mass spectrometry (ICP-MS) after pressure digestion. This method was validated for infant
formula, wheat noodle, cheese, liver, beetroot and cocoa powder at mass fractions in the range of
1 mg/kg to 200 mg/kg. At concentrations above 200 mg/kg, digestion temperatures higher than 220 °C
can be necessary to recover the aluminium as completely as possible.
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 ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
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 http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
Aluminium is determined quantitatively by ICP-MS after digestion of the sample with nitric acid (with
addition of water in case of foods with low water content) according to the pressure digestion process
described in EN 13805 but without the use of hydrofluoric acid. The digestion conditions are chosen in
such a way that even for samples with aluminium compounds of low solubility (e.g. silicates, oxides)
low findings are kept to a minimum.
5 Reagents
The mass concentration of aluminium shall be low enough in the reagents and water not to affect the
results.
All reagents shall be of analytical grade, i.e. pro analysi, p.a. or similar unless otherwise specified.
Use water conforming to grade 2 of EN ISO 3696.
5.1 Nitric acid, mass fraction w = at least 65 %, density = 1,4 g/ml.
5.2 Aluminium stock solution, with a certified mass concentration ρ = 1 000 mg/l.
5.3 Rhodium stock solution, ρ = 1 000 mg/l as internal standard.
The internal standard shall be free from aluminium impurities and shall be present in the sample in
negligibly small amounts only.
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Rhodium and Indium are suitable as internal standards. Other internal standards, especially those
having mass/charge ratios (m/z) < 100, shall not be used, since molecule ion interferences can distort
the measurement.
NOTE The verification of molecule ion interferences was performed in the collaborative study using a high-
1)
resolution ICP mass spectrometer with a resolution of R = 4 000 .
5.4 Standard solutions
5.4.1 General
When preparing solutions special care shall be taken to avoid contaminations. For aluminium there are
various sources of contamination, e.g. volumetric flasks made of glass. Annex B of this document
requires special attention.
5.4.2 Aluminium standard solution 1, ρ = 10 mg/l.
Fill 10 ml of water into a 50-ml volumetric flask; add 2 ml of nitric acid (5.1) and mix. After cooling
down to room temperature, pipette exactly 500 µl of the aluminium stock solution (5.2) to the flask, and
fill up with water to the mark. This standard solution 1 is stable for at least 3 months.
5.4.3 Aluminium standard solution 2, ρ = 1 mg/l.
Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.
After cooling down to room temperature, pipette exactly 5 ml of the aluminium standard solution 1 of
ρ = 10 mg/l (5.4.2) to the flask and fill up with water to the mark. This standard solution 2 is stable for
at least 3 months.
5.4.4 Aluminium standard solution 3, ρ = 0,1 mg/l.
Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.
After cooling down to room temperature, pipette exactly 5 ml of the aluminium standard solution 2 of
ρ = 1 mg/l (5.4.3) and fill up with water to the mark. This standard solution 3 is stable for at least
3 months.
5.4.5 Rhodium standard solution 1 (internal standard solution 1), ρ = 10 mg/l.
Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.
After cooling down to room temperature, pipette exactly 500 µl of the rhodium stock solution (5.3) to
the flask and fill up with water to the mark. This internal standard solution 1 is stable for at least
3 months.
5.4.6 Rhodium standard solution 2 (internal standard solution 2), ρ = 1,0 mg/l.
Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.
After cooling down to room temperature, pipette exactly 5 ml of the rhodium standard solution 1 of
ρ = 10 mg/l (5.4.5) and fill up with water to the mark. This internal standard solution 2 is stable for at
least 3 months.


1) resolution R = m/Δm.
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5.5 Aluminium calibration solutions
The mass concentrations of the calibration solutions described are examples and may be changed
according to the sensitivity of the measuring instrument and the concentration range to be analysed.
Make sure that the calibration is carried out within the linear range of the detector system. For
calibration, at least 3 calibration solutions of different concentrations should be prepared. Make sure
that the acid concentration of the calibration solutions corresponds to the test solution.
In order to avoid contaminations originating from the flask material, do not use volumetric flasks made
from borosilicate glass. Note the information on contaminations provided in B.1.
Prepare the calibration solutions from aluminium standard solution 2 and 3 (5.4.3 and 5.4.4) according
to the following scheme in Table 1:
Table 1 — Example of aluminium calibration solutions
Calibration Volume of aluminium Volume of internal Mass concentration of
solution no standard solution standard solution 2 aluminium in the
(5.4.6) calibration solution
 µl µg/l
1 200 µl of standard solution 3 200 1
(5.4.4)
2 100 µl of standard solution 2 200 5
(5.4.3)
3 500 µl of standard solution 2 200 25
(5.4.3)
4 2000 µl of standard solution 2 200 100
(5.4.3)
EXAMPLE Fill 4 ml to 5 ml of water into a 20 ml volumetric flask, add 250 µl of nitric acid (5.1), and mix.
After cooling down to room temperature, pipette the standard solution and the internal standard solution 2
according to Table 1 to the flask, fill up to the mark with water and mix.
Alternatively, the internal standard can be pumped into the sample flow via a Y-piece during
measurement. In this case, the internal standard solution is not pipetted into the calibration solutions.
NOTE The acid concentration of the calibration solution in the example is adapted to a digestion with 2,5 ml
of nitric acid (5.1), a filling volume of 20 ml and a dilution factor of 10 (in case of a dilution with water).
The calibration solutions shall be freshly prepared each working day.
5.6 Zero-point solution
For the zero-point solution, add 1,25 ml of nitric acid (5.1) and if applicable the internal standard 2 (in
exactly the same mass concentration as in the calibration solutions, according to the example given
in 5.5) to a 100 ml volumetric flask and fill up with water.
6 Apparatus
All equipment and labware that come into direct contact with the sample and the solutions used shall
be carefully pretreated/cleaned according to EN 13804 to minimize the blank value (see Annex B for
details). In addition to standard laboratory equipment, use the following:
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6.1 Inductively coupled plasma mass spectrometer (ICP-MS).
The ICP-MS shall include inductively coupled argon plasma, sample supply and nebulising system as
well as instrument controlling and data acquisition. In order to avoid interferences on the atomic mass
of aluminium, it can be necessary to use a mass spectrometer that is able to delete or minimize
interferences (e.g. which is equipped with cell technology or resolution above 300) [1].
6.2 Digestion vessels, e.g. of polyfluoropolymers or quartz with volumes from 70 ml to 100 ml.
6.3 Test tube shaker, optional.
6.4 Analytical balance, capable to weigh to the nearest milligram.
7 Procedure
7.1 Digestion
7.1.1 General
To ensure complete dissolution of aluminium the following shall be respected:
— ensure that the sample is sufficiently homogeneous;
— in case of incomplete digestion or high aluminium contents, it may be beneficial to use a test
portion as small as possible (at least 200 mg for dry samples) in order to digest aluminium
compounds as completely as possible;
— for samples containing silicates, digestion temperatures above 220 °C may be necessary in order to
dissolve the aluminium as completely as possible;
— in case of samples with low water content, first add water and mix intensively, before adding
concentrated nitric acid;
— do not use hydrogen peroxide for digestion.
Further information regarding test portions and digestion are given in B.2 and B.3.
For pressure digestion according to EN 13805, different vessels may be used depending on the
instrument type and manufacturer. The maximum test portion and the minimum liquid volume depend
on the pressure stability of the respective vessels. The specifications according to 7.1.2 refer to
digestion vessels with volumes from 70 ml to 100 ml and a minimum liquid volume of 5 ml.
All indications in 7.1.2 shall be adjusted to the digestion instrument used. For safety reasons the
manufacturer's specifications shall be strictly followed.
7.1.2 Digestion procedure
Before digestion, different amounts of water, depending on the different types of food [2], are added in
order to obtain comparable acid concentrations in the final digestion solution. The amount of water to
be added depends on the test portion and thus on the content of carbon and water in the food type.
Add just as much water to the initial test portion that is necessary to suspend the food completely. Then
complete the test portion with water to reach 3 g. Water is also added to fat-containing foods, even if a
suspension is hardly possible.
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Example for digestion of powdery food: Add 2,5 ml of water to the dry food, e.g. 0,5 g of flour. Mix the
contents of the digestion vessel intensively, e.g. on a test-tube shaker. Repeat shaking every 10 min to
15 min until the susp
...