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

This European Standard specifies a method for the determination of trace elements, heavy metals and other elements in animal feed by ICP-MS. The method is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after pressurised digestion. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described is suitable for use in quadrupole instruments equipped either with or without additional technology to reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution sector-field systems.
The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. High-resolution sector-field ICP-MS was not tested in the validation ring trial.
The limit of quantification for each element is dependent on the sample matrix as well as the instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg and As 0,05 mg/kg should normally be quantifiable.
Details on the successfully tested working range for each element are described in this standard.

Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Spurenelementen, Schwermetallen und anderen Elementen in Futtermitteln mittels ICP-MS (Multimethode)

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Spurennährstoffen, Schwermetallen und anderen Elementen in Tierfuttermitteln durch Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) fest. Das Verfahren wird zur Bestimmung von As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U und Zn in der Extraktionslösung nach Druckaufschluss verwendet. Zur Bestimmung von extrahierbarem Blei in Mineralstoffen und Futtermitteln, die Schichtsilikate enthalten (z. B. kaolinitischer Ton), sollte Nassaufschluss mit Salpetersäure verwendet werden. Das beschriebene Verfahren ist zur Verwendung mit Quadrupol Instrumenten geeignet, die entweder mit oder ohne zusätzliche Technologien zur Reduzierung der Interferenzen von Molekülionen (z. B. Kollisions  oder Reaktionstechnologien) sowie hochauflösende Sektorfeldsysteme ausgestattet sind.
Das Verfahren wurde vollständig im Rahmen eines Ringversuches mit acht Futtermittelproben für die Elemente As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U und Zn statistisch geprüft und bewertet. Für Elemente mit einem HorRat Wert höher als 2 (z. B. Quecksilber, siehe Anhang A) ist das Verfahren eher als Screening Verfahren und nicht für Bestätigungszwecke geeignet Eine ICP MS mit hochauflösendem Sektorfeldsystem wurde im Rahmen des Ringversuches nicht geprüft.
Die Nachweisgrenze des Verfahrens hängt bei jedem Element sowohl von der Probenmatrix als auch vom verwendeten Gerät ab. Für die Elemente Co, Mn, Mo, Pb, Tl und U sollte eine Bestimmungsgrenze von 0,10 mg/kg, für die Elemente Fe und Zn 5,0 mg/kg, für Cd 0,03 mg/kg, für Hg 0,04 mg/kg und für As 0,05 mg/kg üblicherweise quantifizierbar sein.
Nähere Angaben zu den erfolgreich geprüften Arbeitsbereichen für jedes Element werden in dieser Norm beschrieben.

Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Dosage par ICP-MS (multiméthode) des éléments traces, métaux lourds et autres éléments inorganiques présents dans les aliments

Krma: metode vzorčenja in analize - Določevanje elementov v sledovih, težkih kovin in drugih elementov v krmi z ICP-MS (večelementna metoda)

Ta evropski standard določa metodo za določanje elementov v sledovih, težkih kovin in drugih elementov v živalski krmi po ICP-MS. Metoda se uporablja za določanje As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U in Zn v raztopini za izločanje po razgradnji pod tlakom. Za določevanje izločljivega svinca v mineralih in krmah, ki vsebujejo filosilikate (npr. kaolinitna glina), je treba uporabiti postopek mokrega razklopa z dušikovo kislino. Opisana metoda je primerna za uporabo pri kvadrupolnih instrumentih, opremljenih z dodatno tehnologijo za zmanjševanje motenj molekularnih ionov (npr. tehnologije trkov ali reakcij) ali brez te tehnologije, ter pri visokoločljivostnih sistemih sektorskih polj.
Metoda je bila v celoti statistično preskušena in ocenjena v medlaboratorijskem poskusu, sestavljenem iz osmih vzorcev živalske krme za elemente As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U in Zn. Visokoločljivostni ICP-MS za sektorsko polje ni bil preskušen pri primerjalnem preskusu za validacijo.
Meja kvantifikacije vseh elementov je odvisna od matrice vzorca in instrumenta. Pri elementih Co, Mn, Mo, Pb, Tl, U naj bi se običajno pridobila meja kvantifikacije 0,10 mg/kg, za elementa Fe in Zn 5,0 mg/kg, za Cd pa naj bi se običajno pridobila meja 0,03 mg/kg, za Hg 0,04 mg/kg in za As 0,05 mg/kg.
Podrobnosti o uspešno preskušenem delovnem razponu za posamezen element so opisane v tem standardu.

General Information

Status
Published
Public Enquiry End Date
19-Dec-2016
Publication Date
12-Feb-2018
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
02-Feb-2018
Due Date
09-Apr-2018
Completion Date
13-Feb-2018

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SLOVENSKI STANDARD
SIST EN 17053:2018
01-marec-2018
.UPDPHWRGHY]RUþHQMDLQDQDOL]H'RORþHYDQMHHOHPHQWRYYVOHGRYLKWHåNLK
NRYLQLQGUXJLKHOHPHQWRYYNUPL],&306 YHþHOHPHQWQDPHWRGD
Animal feeding stuffs: Methods of sampling and analysis - Determination of trace
elements, heavy metals and other elements in feed by ICP-MS (multi-method)
Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von

Spurenelementen, Schwermetallen und anderen Elementen in Futtermitteln mittels ICP-

MS (Multimethode)

Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Dosage par ICP-MS

(multiméthode) des éléments traces, métaux lourds et autres éléments inorganiques

présents dans les aliments
Ta slovenski standard je istoveten z: EN 17053:2018
ICS:
65.120 Krmila Animal feeding stuffs
SIST EN 17053:2018 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 17053:2018
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SIST EN 17053:2018
EN 17053
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2018
EUROPÄISCHE NORM
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of trace elements, heavy metals and other
elements in feed by ICP-MS (multi-method)

Aliments des animaux - Méthodes d'échantillonnage et Futtermittel - Probenahme- und

d'analyse - Dosage par ICP-MS (multiméthode) des Untersuchungsverfahren - Bestimmung von

éléments traces, métaux lourds et autres éléments Spurenelementen, Schwermetallen und anderen

inorganiques présents dans les aliments Elementen in Futtermitteln mittels ICP-MS

(Multimethode)
This European Standard was approved by CEN on 27 November 2017.

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, 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 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

© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17053:2018 E

worldwide for CEN national Members.
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SIST EN 17053:2018
EN 17053:2018 (E)
Contents Page

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Principle ............................................................................................................................................................. 4

4 Reagents ............................................................................................................................................................. 5

5 Apparatus ........................................................................................................................................................... 6

6 Sampling ............................................................................................................................................................. 6

7 Preparation and preservation of test samples ..................................................................................... 6

7.1 General ................................................................................................................................................................ 6

7.2 Animal feeding stuff, which can be ground as such ............................................................................ 7

7.3 Mineral animal feeding stuffs ..................................................................................................................... 7

8 Procedure........................................................................................................................................................... 7

8.1 Pressure digestion .......................................................................................................................................... 7

8.2 Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay)

– extraction with diluted nitric acid ......................................................................................................... 7

8.3 Calibration ......................................................................................................................................................... 8

8.4 Preparation of measurement solutions .................................................................................................. 8

8.5 Determination .................................................................................................................................................. 9

8.6 Quality assurance ......................................................................................................................................... 12

9 Calculation ...................................................................................................................................................... 12

10 Precision .......................................................................................................................................................... 13

10.1 General ............................................................................................................................................................. 13

10.2 Repeatability .................................................................................................................................................. 13

10.3 Reproducibility ............................................................................................................................................. 13

11 Test report ...................................................................................................................................................... 13

Annex A (informative) Statistical results of interlaboratory tests (listed by element) ................... 14

Annex B (informative) Interferences ................................................................................................................. 27

B.1 Interferences in ICP-MS ............................................................................................................................. 27

B.2 Technical solutions to overcome interferences ................................................................................ 28

Bibliography ................................................................................................................................................................. 29

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SIST EN 17053:2018
EN 17053:2018 (E)
European foreword

This document (EN 17053:2018) has been prepared by Technical Committee CEN/TC 327 “Animal

feeding stuffs - Methods of sampling and analysis”, the secretariat of which is held by NEN.

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 July 2018, and conflicting national standards shall be

withdrawn at the latest by July 2018.

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.

This document has been prepared under a mandate given to CEN by the European Commission and the

European Free Trade Association.

WARNING — The method described in this standard implies the use of reagents that pose a

hazard to health. The standard does not claim to address all associated safety problems. It is the

responsibility of the user of this standard to take appropriate measures for the health and safety

protection of the personnel prior to use of the standard and to ensure that regulatory and legal

requirements are complied with.

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.
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SIST EN 17053:2018
EN 17053:2018 (E)
1 Scope

This European Standard specifies a method for the determination of trace elements, heavy metals and

other elements in animal feed by inductively coupled plasma mass spectrometry (ICP-MS). The method

is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after

pressurized digestion. For the determination of extractable lead in minerals and feeds containing

phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described

is suitable for use in quadrupole instruments equipped either with or without additional technology to

reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution

sector-field systems.

The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal

feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. For elements

with a HORRAT value higher than 2 (e.g. mercury, see Annex A) the method is more applicable as a

screening method and not for confirmatory purposes. High-resolution sector-field ICP-MS was not

tested in the validation ring trial.

The limit of quantification for each element is dependent on the sample matrix as well as the

instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should

normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg

and As 0,05 mg/kg should normally be quantifiable.

Details on the successfully tested working range for each element are described in this standard.

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 ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)

EN ISO 6498, Animal feeding stuffs — Guidelines for sample preparation (ISO 6498)

3 Principle

For the determination of As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn a test portion of the sample is

digested with concentrated nitric acid under pressure.

For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite

clay) wet digestion with nitric acid should be used.

The concentration of the elements is determined by inductively coupled plasma mass spectrometry

(ICP-MS) using external calibration or standard addition technique. To reduce occurring mass

interferences mathematical correction equations, physical or chemical technical solutions (see B.2) or

high-resolution sector-field ICP-MS may be applied.
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SIST EN 17053:2018
EN 17053:2018 (E)
4 Reagents

WARNING — The use of this European Standard can involve hazardous materials, operations

and equipment. This standard does not purport to address all the safety problems associated

with its use. It is the responsibility of the user of this European Standard to establish

appropriate safety and health practices and determine the applicability of regulatory limitations

prior to use.

Use only reagents of recognized analytical grade and water conforming to grade 2 of EN ISO 3696.

4.1 Nitric acid concentrated, not less than 65 % (mass fraction), c(HNO ) = 14,4 mol/l, having a

density of approximately ρ(HNO ) = 1,40 g/ml.

4.2 Nitric acid solution of 5 % (mass fraction), Pipette 54 ml of nitric acid (4.1) into a 1 000 ml

volumetric flask (5.4) and fill to the mark with water.

4.3 Nitric acid solution (rinsing solution), Pipette 20 ml nitric acid (4.1) in a 1 000 ml volumetric

flask (5.4). Fill up to the mark with water.

4.4 Hydrochloric acid concentrated, 30 % (mass fraction), c(HCl) = 9,5 mol/l, having a density of

approximately ρ(HCl) = 1,15 g/ml.

4.5 Hydrogen peroxide, not less than 30 % (mass fraction), c(H O ) = 9,7 mol/l, having a density

2 2
of approximately ρ(H O ) = 1,12 g/ml.
2 2

4.6 Single-element and multi-element stock solutions for ICP-MS, β = 1 000 mg/l, It is advisable

to use certified multi-element stock solutions. Stock solutions with concentrations different from

1 000 mg/l may be used as well. Stock solutions are considered to be stable for several months.

4.7 Calibration solutions, The concentrations of the calibration solutions depend on the element and

the estimated concentration levels in the samples. When preparing calibration solutions care should be

taken to pipette suitable volumes, intermediate dilution steps are recommended. If calibration solutions

are prepared from single-element stock solutions, it should be checked whether they are chemically

compatible and sufficiently pure (specification). Calibration solutions shall be prepared daily.

4.8 Internal standard stock solution, β = 1000 mg/l; As internal standard rhodium is

recommended.

NOTE Alternatively, for low mass elements germanium, it is advised to use indium or scandium as internal

standards. Rhenium, thulium and lutetium are beneficial for the quantification of high mass elements.

4.9 Internal standard working solution, β = 1 mg/l, Dilute 1 ml of the internal standard stock

solution (4.8) to 1 000 ml with water.
4.10 Gold chloride stock solution, AuCl (in 10 % HCl), β = 10 g Au/l.

4.11 Gold stability solution, β = 200 mg Au/l, Place 200 ml of water into a 500 ml volumetric flask

(5.4), pipette 250 ml conc. HCl (4.4) and 10,0 ml gold chloride stock solution (4.10) and fill to the mark

with water.
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SIST EN 17053:2018
EN 17053:2018 (E)
5 Apparatus
Usual laboratory apparatus and, in particular, the following:
5.1 Laboratory grinder

5.1.1 Laboratory grinder, capable of grinding to a particle size of less than or equal to 0,5 mm, e.g. a

knife mill or equivalent.

5.1.2 Laboratory grinder, capable of grinding to a particle size of less than or equal to 0,1 mm, e.g. a

ball mill or equivalent.

Check that the mill used does not influence the concentration of elements in the sample (e.g. adsorption,

contamination) which shall be analysed.
5.2 Analytical balance, capable of weighing to an accuracy of 1 mg.

5.3 Pressure digestion apparatus, capable to reach temperatures above 210 °C. The apparatus shall

be tested for safety pressure vessels made of acid-resistant materials and having vials for the sample of

acid-resistant material with low level of contamination by elements to be determined. Instead of

polytetrafluoroethylene (PTFE) vials, it is better to use graduated quartz vials, fluorinated ethylene

propylene (FEP) vials or perfluoroalkoxy (PFA) vials. Quartz is advisable to be used for decomposition

temperatures above 230 °C.
NOTE The use of a microwave heated pressure digestion apparatus is an option.
5.4 One-mark volumetric flasks;
5.5 Inductively Coupled Plasma Mass Spectrometer (ICP-MS);

5.6 Freeze-drying equipment, capable of freeze-drying liquid animal feeding stuffs;

5.7 Oven for pre-drying, capable to hold a temperature of 70 °C ± 5 °C;
5.8 Beaker, capacity 250 ml;
5.9 Electric hot plate, with temperature control.
6 Sampling

Sampling is not part of the method specified in this European Standard. A recommended sampling

method is given in EN ISO 6497. It is important that the laboratory receives a sample which is truly

representative and has not been damaged or changed during transport or storage.
7 Preparation and preservation of test samples
7.1 General
Prepare the test sample in accordance with EN ISO 6498:

— The grinding shall be done in conditions such that the substance is not appreciably heated and that

no contamination takes place by the grinding tools;

— The operation shall be repeated as many times as is necessary and it shall be performed as quick as

possible in order to prevent any gain or loss of constituents (water);
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SIST EN 17053:2018
EN 17053:2018 (E)

— The whole ground product is placed in a flask made of e.g. polypropylene, which can be stoppered

and stored in such way to prevent any change in composition;

— Before any weighing is carried out for the analysis, the whole test sample shall be thoroughly mixed

for reasons of homogeneity. Since a maximum of 0,5 g of sample is used for the digestion it is of the

utmost importance to have a homogeneous sample in order to take a representative sub sample.

7.2 Animal feeding stuff, which can be ground as such

Grind the laboratory sample (usually 500 g), using a laboratory grinder (5.1) or mortar, until a particle

size of 0,5 mm or less has been reached.
7.3 Mineral animal feeding stuffs

Mineral compounds, except mineral products containing crystalline water, e.g. MgCl ⋅6HO, shall be

2 2

ground using a laboratory grinder (5.1.2) or mortar until a particle size of 0,1 mm or less has been

reached. Mineral products containing crystalline water such as phyllosilicates should not be ground.

8 Procedure
8.1 Pressure digestion
8.1.1 General

Match the initial sample mass to the capacity of the digestion vessel, with the manufacturer's

instructions being strictly followed for safety reasons.
8.1.2 Example of a high pressure digestion

When using a 100 ml vial, weigh about 0,5 g of the prepared test sample to the nearest 1 mg. Add 3 ml

of nitric acid (4.1) and seal the digestion vial and the pressure vial in the correct manner. Leave to pre-

digest for about 30 min and heat it in a pressure digestion apparatus (5.3) from room temperature to

150 °C in 60 min, then to at least 210 °C in 40 min and keep this temperature for 90 min before cooling

down. Dilute the digestion solution accordingly with water. Treat a blank in the same way.

8.1.3 Example of microwave digestion

When using 100 ml vials, weigh about 0,5 g of the prepared test sample to the nearest 1 mg. Add 3 ml of

nitric acid (4.1) and 0,5 ml of hydrogen peroxide (4.5), seal the digestion vial and the pressure holders

in the correct manner. Leave to pre-digest outside the microwave oven (5.3) for about 30 min. Apply

low microwave energy at the beginning of the digestion and slowly raise the energy to the maximum

power, to reach at least 210 °C. Hold this temperature for at least 20 min, cool down for minimum

20 min to 25 min. Dilute the digestion solution accordingly with water. Treat a blank in the same way.

8.2 Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay)

– extraction with diluted nitric acid

Weigh about 2 g of the prepared test sample to the nearest 1 mg into a beaker of 250 ml (5.8). Add

85 ml diluted nitric acid (4.2). Cover the beaker with a watch-glass and boil for 30 min on a hot plate

(5.9). Allow to cool. Transfer the liquid into a 100 ml volumetric flask (5.4), rinse the beaker and the

watch-glass several times with water. Dilute to the mark with water. After homogenizing, filter through

a dry folded filter paper into a dry conical flask. Use the first portion of the filtrate to rinse the glassware

and discard that part. If the determination is not carried out immediately, the conical flask with the

filtrate shall be stoppered. Treat a blank in the same way.
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SIST EN 17053:2018
EN 17053:2018 (E)
8.3 Calibration
8.3.1 General

The concentration of elements in the extraction solution is quantified against element calibration

solutions (4.7) by means of external calibration or standard addition technique.

Usually, there exists a stable linear relationship over several decimal powers between the signal

measured by the detector and the concentration of elements in the analyte solution.

8.3.2 External calibration

For the calibration at least five calibration solutions are recommended, of which one is a blank

calibration solution. Due to different element concentrations in the feeding stuff the calibration range is

to adjust, considering the resulting count rate. If the linearity of the calibration is proved, further a two-

point-calibration, of which one is a blank solution, is allowed.

Appropriate matrix matching at least in acid composition and concentration of the calibration solutions

to that of the sample solutions shall be performed if an external calibration method is used.

8.3.3 Standard addition technique

The standard addition curve should consist of at least four points, of which three are additions. For

those elements whose concentration is near the limit of quantification, the standard addition curve

should consist of at least three points, of which two are additions. If three additions are used, the

concentration of the highest standard should be 3 to 5 times the concentration in the sample solution.

8.4 Preparation of measurement solutions
8.4.1 General

The element concentrations in feed can vary in a wide range. Therefore suitable dilution steps of the

sample solutions, obtained from the pressure digestion (8.1) or extraction procedure (8.2), can be

necessary. The sample solutions should be diluted to a level that ensures that the salt concentration in

the measuring solutions is below 0,2 %.

Internal standard (4.9) is added to all measuring solutions taking care that the resultant concentration

of internal standard is matched in all solutions (e.g. β = 10 µg/l). Alternatively, it may be worthwhile to

add the internal standard online during measurement.

NOTE 1 Measurements in HR-ICP-MS systems generally use lower concentrations of internal standard (e.g.

β = 1 µg/l).

NOTE 2 To reduce matrix effects it can be worthwhile to assay higher dilution steps when adequate system

sensitivity and clean lab environment are ensured (low blanks). If using HR-ICP-MS systems higher dilutions are

required to achieve lower salt concentrations (e.g. ≤ 0,05 %).
8.4.2 Mercury

If the determination of mercury is desired, an additional activity is needed to prevent both mercury

adsorption to surfaces and memory effects. An effective method is to increase the concentration of HCl

to 0,5 or 1 % in all measuring solutions by adding the appropriate volume of HCl (4.4).

Another possible activity to prevent adsorption is the addition of gold (4.11) to all measuring solutions.

Every solution should contain a gold concentration of at least c = 0,2 mg Au/l.
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SIST EN 17053:2018
EN 17053:2018 (E)
8.5 Determination
8.5.1 ICP-MS Optimization

The ICP-MS system is optimized and checked in accordance with the instructions given by the supplier’s

user manual. In doing so, care should be taken to ensure that system sensitivity and signal stability are

adequate. With quadrupole-equipped mass spectrometers, the rate of both oxide ions and double

charged ions formation should be kept below 3 % and held as constant as possible. With sector-field

high-resolution ICP-MS systems adequate resolution shall be ensured.

To avoid memory effects, the nebulizer is thoroughly rinsed with a rinsing solution (4.3).

It is recommended to check by control measurements on a blank whether the purging time selected is

appropriate following the analysis of a sample solution.
8.5.2 Interferences

Interferences in ICP-MS are caused when ions generated from the plasma, the sample, or a combination

of the two carry a mass-to-charge ratio that is identical to that of the analyte ion. A short description of

interferences and a survey of techniques for lowering are shown in Annex B.
8.5.3 Analyte isotopes

Table 1 shows recommended analyte isotopes, selected isobaric and molecular ion interferences and

recommended techniques.
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SIST EN 17053:2018
EN 17053:2018 (E)

Table 1 — Recommended analyte isotopes, selected isobaric and molecular ion interferences

and recommended techniques
Recommended technique to
Element Isotope Interferenced by
overcome interferences
75 40 35 + 40 35 + 36 39 + 59 16 + 35 37
As Ar Cl , Ca Cl , Ar K , Co O Math. Corr. ( Cl/ Cl), KED, RM
91 91 + 75 16 + 90
( AsO) Zr RM ( As O ), Math. Corr. ( Zr)
111 95 16 + 94 16 1 + 94 16 1 +
Cd Cd Mo O , Mo O H , Zr O H KED, RM
112 112 + 96 16 + 118
Cd Cd Sn , Ru O Math. Corr. ( Sn), KED, RM
114 114 + 98 16 + 98 16 + 118
Cd Cd Sn , Mo O , Ru O Math. Corr. ( Sn), KED, RM
43 16 + 42 16 1 + 24 35 +
Ca O , Ca O H , Mg Cl ,
59 43
Co Co Math. Corr. ( Ca), KED, RM
36 23 + 40 18 1 +
Ar Na , Ar O H
40 23 + 31 16 16 + 26 37 + 47 16 +
Ar Na , P O O , Mg Cl , Ti O ,
Cu Cu KED
40 23 +
Ca Na
65 130 2+ 49 16 + 40 25 +
Cu Cu Ba , Ti O , Ar Mg KED
56 40 16 + 40 16 +
Fe Fe Ar O , Ca O KED, RM
201 184 16 1 + 185 16 +
Hg Hg W O H , Re O
55 40 14 1 + 40 15 +
Mn Mn Ar N H , Ar N KED
95 40 39 16 +
Mo Ar K O KED
98 98 + 41 41 16 + 101
Mo Ru , K K O Math. Corr. ( Ru), KED
206
measure all three isotopes and sum
207
the signal intensities
208
78 78 + 38 40 + 38 40 + 156 2+ 83
Se Kr , Ar Ar , Ar Ca , Gd Math. Corr. ( Kr), KED, RM
80 80 + 40 40 + 40 40 + 83
Se Se Kr , Ar Ar , Ar Ca Math. Corr. ( Kr), KED, RM
82 82 + 12 35 35 + 83 35
Se Kr , C Cl Cl Math. Corr. ( Kr, Cl), KED, RM
205
Tl Tl
238
U U
66 50 16 + 32 34 + 34 16 16 + 32 16 18 +
Zn Ti O , S S , S O O , S O O KED
34 34 + 34 16 18 + 32 18 18 + 40 14 14 +
S S , S O O S O O , Ar N N ,
Zn KED
36 32 +
Ar S
KED – Kinetic Energy Discrimination; RM – Reaction Mode.
---------------------- Page: 12 ----------------------
SIST EN 17053:2018
EN 17053:2018 (E)

Table 2 shows recommended analyte isotopes and resolution levels for High-Resolution-ICP-MS.

Table 2 — Recommended analyte isotopes and resolution levels for HR-ICP-MS
Analyte Isotope Mass [amu] Resolution Interference by
As As 74,9211 High
95 16 +
Mo O ,
111
Cd Cd 110,9033 Low
94 16 1 +
Mo O H
Co Co 58,9332 Medium
Cu Cu 62,9291 Medium
Fe Fe 55,9344 Medium
Mn Mn 54,9380 Medium
Mo Mo 97,9049 Low
206
Pb 205,9739
207
Pb Pb 206,9753 Low
208
Pb 207,9761
Se Se 76,9211 High
Zn Zn 65,9260 Medium
8.5.4 Working range

Table 3 shows the tested working ranges. The working ranges may be extended provided that further

in-house validation has been carried out.
Table 3 — Tested working ranges
Tested working range
Lowest concentration Highest concentration
Element
[mg/kg] [mg/kg]
As 0,08 20
Cd 0,03 12
Co 0,30 62
Cu 2,50 1 390
Fe 36 540
Hg 0,04 11
Mn 12 4 600
Mo 0,30 8
Pb 0,12 15
Se 0,40 13
Tl 0,01 10
U 0,08 145
Zn 55 6 300
---------------------- Page: 13 ----------------------
SIST EN 17053:2018
EN 17053:2018 (E)
8.6 Quality assurance

Blank and control samples are measured at regular intervals to verify extraction and calibration.

Certified reference materials, material from former proficiency tests or well characterized in-house

reference materials can be used as control samples. At least one suitable control sample (sample matrix

should be as similar as possible to sample to be analysed) and one blank have to carry through the

entire analysis for each sample series. The concentration of analyte in the control sample shall be

sufficiently different from the limit of quantification.

Accuracy is verified by certified reference material. The analytical value should be within two standard

deviations of reproducibility.

Reproducibility is determined using control charts of the mean. The results should be within two

standard deviations of repeatability.
9 Calculation

The mass fractions of the elements analysed in the original sample are calculated from the calibration

function using sample mass, final volume and dilution factor.
Calibration function
I b x β+a (1)
St St
Equation
II−−a
[ ] VF ×
Sa Bl
w × (2)
where
𝛽𝛽 is the concentration of the standard, in mg/l
...

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