SIST EN 10355:2014

Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination of Si, Mn, P, Cu, Ni, Cr, Mo, Sn and Al (soluble) [Routine method]

This European Standard specifies an inductively coupled plasma optical emission spectrometry routine method for the analysis of unalloyed and low alloyed steels, whose iron content shall be at least 95 %. This standard differs from the similar standard EN 10351:2011 in that it is optimised for the determination of silicon.
This method is applicable to the elements listed in Table 1 within the ranges shown.
The sample preparation described may not completely dissolve samples having a combination of high chromium and substantial carbon. Incomplete dissolution may also affect the determination of manganese and molybdenum in these samples. For this reason, the scope of the method is limited to chromium contents = 0,9 %, whereas the scope of EN 10351 covers a range of up to 1,6 % chromium.
Table 1 - Application ranges
Element   Mass fraction %
   min.   max.
Si   0,020   0,45
Mn   0,005   1,40
P   0,005   0,10
Cu   0,005   0,60
Ni   0,010   2,00
Cr   0,010   0,90
Mo   0,005   0,60
Sn   0,010   0,10
NOTE   For tin, see NOTE 2 under Clause 11.
In all cases, the ranges specified can be extended or adapted (after validation) for the determination of other mass fractions, provided that the iron content in the samples under concern is above 95 %.
Other elements may be included. However such elements and their mass fractions should be carefully checked, taking into account the possible interferences, the sensitivity, the resolution and the linearity criteria of each instrument and each wavelength.
Depending also on the sensitivity of each instrument, suitable dilutions of the calibration and the test sample solutions may be necessary.
Moreover, even if the method described is "multi elemental", it is not absolutely necessary to carry out the determination of all the elements of its scope simultaneously. The measurement conditions have to be optimised by each laboratory, depending on the performances of each apparatus available.

Chemische Analyse von Eisenwerkstoffen - Analyse von unlegierten und niedrig legierten Stähle mittels optischer Emissionsspekrometrie mit indukiv gekoppeltem Plasma - Bestimung von Si, Mn, P, Cu, Ni, Cr, Mo, Sn und Al (lösung) [Routineverfahren]

Diese Europäische Norm legt ein Verfahren der optischen Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP Emissionsspektrometrie) fest, das routinemäßig zur Analyse unlegierter und niedrig legierter Stähle anzuwenden ist, die einen Eisengehalt von mindestens 95 % haben. Diese Norm weicht von der Norm EN 10351:2011 ab; EN 10351:2011 ist für die Bestimmung von Si optimiert.
Das Verfahren ist auf die in Tabelle 1 aufgeführten Elemente innerhalb der angegebenen Bereiche anwendbar.
Die beschriebene Herstellung von Proben kann Proben, die sich aus einem hohen Chrom- und erheblichem Kohlenstoff¬gehalt zusammensetzen, nicht vollständig lösen. Diese unvollständige Lösung kann außerdem die Bestimmung von Mangan sowie Molybdän in diesen Proben beeinflussen. Aus diesem Grund ist der Anwendungsbereich dieses Verfahrens auf einen Chromanteil von  0,9 % beschränkt, wogegen der Anwendungsbereich der EN 10351 einen Bereich  1,6 % Cr abdeckt.
Tabelle 1 — Anwendungsbereiche
Element   Massenanteil
%
   min.   max.
Si   0,020   0,45
Mn   0,005   1,40
P   0,005   0,10
Cu   0,005   0,60
Ni   0,010   2,00
Cr   0,010   0,90
Mo   0,005   0,60
Sn   0,010   0,10
ANMERKUNG   Für Zinn siehe Absatz 11, Anmerkung 2.
Alle angegebenen Bereiche können erweitert oder (nach einer Validierung) so angepasst werden, dass auch andere Massenanteile zu bestimmen sind, sofern die zu analysierenden Proben einen Eisenanteil von mehr als 95 % haben.
Das Verfahren darf auch dann angewendet, wenn weitere Elemente enthalten sind. Diese Elemente und ihre Massenanteile sollten jedoch unter Berücksichtigung möglicher Störungen, der Empfindlichkeit, der Auflösung und der Linearitätskriterien für jedes ICP Emissionsspektrometer und für jede Wellenlänge sorgfältig überprüft werden.
Entsprechend der Empfindlichkeit des jeweiligen ICP Emissionsspektrometers kann es notwendig sein, geeignete Verdünnungen der Kalibrier  und der Untersuchungsprobenlösungen anzuwenden.
Obwohl das beschriebene Verfahren zur „Mehrelementbestimmung“ angewendet wird, müssen nicht unbedingt alle im Anwendungsbereich angegebenen Elemente gleichzeitig bestimmt werden. Die Mess¬bedingungen sind in jedem Prüflaboratorium in Abhängigkeit von den Leistungsparametern der verfügbaren Prüfgeräte zu optimieren.

Analyse chimique des matériaux sidérurgiques - Analyse des aciers non alliés et faiblement alliés par spectrométrie d'émission optique avec source à plasma induit - Détermination de Si, Mn, P, Cu, Ni, Cr, Mo, Sn et Al (soluble) [Méthode de routine]

La présente Norme européenne spécifie une méthode de routine, par spectrométrie d'émission optique avec source à plasma induit, pour l’analyse des aciers non alliés et faiblement alliés ayant une teneur en fer d’au moins 95 %. La présente norme diffère de la norme similaire EN 10351:2011 dans la mesure où elle est optimisée pour la détermination du silicium.
Cette méthode s’applique aux éléments listés dans le Tableau 1, dans les domaines de teneur indiqués.
La préparation d’échantillon décrite ne peut pas conduire à la mise en solution complète d’échantillons ayant à la fois une teneur élevée en chrome et une teneur substantielle en carbone. Cette mise en solution incomplète peut aussi affecter les déterminations du manganèse et du molybdène dans ces échantillons. Pour cette raison, le domaine d’application de la méthode est limité aux teneurs en chrome  0,9 %, alors que le domaine d’application de l’EN 10351 couvre un domaine allant jusqu’à 1,6 % de chrome.
Tableau 1 — Domaines d’application
Elément   Teneur (fraction en masse) %
   min.   max.
Si   0,020   0,45
Mn   0,005   1,40
P   0,005   0,10
Cu   0,005   0,60
Ni   0,010   2,00
Cr   0,010   0,90
Mo   0,005   0,60
Sn   0,010   0,10
NOTE   Pour l’étain, voir NOTE 2 à l’Article 11.
Dans tous les cas, les domaines spécifiés peuvent être étendus ou adaptés (après validation) pour la détermination d’autres teneurs, à condition que la teneur en fer des échantillons concernés soit supérieure à 95 %.
D'autres éléments peuvent être inclus. Il convient toutefois de contrôler, avec la plus grande attention, ces éléments et leurs teneurs, en tenant compte des interférences éventuelles, de la sensibilité, de la résolution et des critères de linéarité de chaque instrument et chaque longueur d'onde.
Aussi, en fonction de la sensibilité de chaque instrument, des dilutions appropriées des solutions d’étalonnage et des solutions d’échantillon peuvent être nécessaires.
En outre, même si la méthode décrite est « multiélémentaire », il n’est pas absolument nécessaire de déterminer simultanément tous les éléments de son domaine d’application. Les conditions de mesurage doivent être optimisées par chaque laboratoire, en fonction des performances de chaque appareil disponible.

Kemična analiza železovih zlitin - Analiza nelegiranih in malolegiranih jekel z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo - Določevanje Si, Mn, P, Cu, Ni, Cr, Mo, Sn in topnega Al [rutinska metoda]

Ta evropski standard določa rutinsko metodo za analizo nelegiranih in malolegiranih jekel z optično emisijsko spektrometrijo z induktivno sklopljeno plazmo, pri čemer mora biti vsebnost železa v jeklu vsaj 95 %. Ta standard se od podobnega standarda EN 10351:2011 razlikuje v tem, da je optimiziran za določevanje silicija. Ta metoda se uporablja za elemente iz preglednice 1 v prikazanih razponih. Z opisano pripravo vzorca se morda vzorci s kombinacijo visoke vsebnosti kroma in znatne vsebnosti ogljika ne bodo raztopili v celoti. Nepopolno raztapljanje lahko vpliva tudi na določevanje mangana in molibdena v teh vzorcih. Zato je področje uporabe metode omejeno na vsebnost kroma ≤ 0,9 %, medtem ko področje uporabe standarda EN 10351 zajema razpon do vključno 1,6 % kroma.

General Information

• Status: Published
• Publication Date: 12-Dec-2013
• ICS: 77.040.30 - Chemical analysis of metals
• ICS: 77.080.20 - Steels
• Technical Committee: IFEK - Ferrous metals
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 05-Dec-2013
• Due Date: 09-Feb-2014
• Completion Date: 13-Dec-2013
• Ref Project: EN 10355:2013 - Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination of Si, Mn, P, Cu, Ni, Cr, Mo and Sn, following dissolution with nitric and sulphuric acids [Routine method]

Overview

EN 10355:2013 specifies a routine ICP‑OES (inductively coupled plasma optical emission spectrometry) method for the chemical analysis of unalloyed and low‑alloy steels (iron ≥ 95 %). The procedure is optimised for silicon (Si) determination and covers dissolution of samples by a nitric‑sulphuric acid mixture followed by oxidation (ammonium peroxodisulphate, H2O2), dilution and ICP‑OES measurement. The standard is intended for routine laboratory use and defines sample preparation, calibration, measurement and expression of results for multiple trace and minor elements.

Key Topics

• Scope & limits
  • Applicable to steels with iron content ≥ 95 %
  • Chromium limited to ≤ 0.90 % (incomplete dissolution and interferences may occur at higher Cr)
• Elements and application ranges
  • Si: 0.020–0.45 %
  • Mn: 0.005–1.40 %
  • P: 0.005–0.10 %
  • Cu: 0.005–0.60 %
  • Ni: 0.010–2.00 %
  • Cr: 0.010–0.90 %
  • Mo: 0.005–0.60 %
  • Sn: 0.010–0.10 %
• Sample dissolution
  • Nitric‑sulphuric acid digestion, followed by ammonium peroxodisulphate boiling and hydrogen peroxide treatment
  • Protocols provided for automated open microwave systems and manual hotplate procedures
  • Advises additions (e.g., HCl) to minimize hydrolysis of Si and Sn and notes potential incomplete dissolution with high Cr + C samples
• Instrumentation & calibration
  • ICP‑OES with appropriate nebulisation; performance criteria suggested in Annex A
  • Use of class A volumetric glassware; internal standard (e.g., Sc or Y) optional
  • Calibration solutions and dilutions must be validated per instrument sensitivity, resolution and linearity
• Quality & precision
  • Clauses on precision, calibration process, reporting and recommended checks to ensure routine accuracy

Applications

• Who uses it
  • Metallurgical and steel production quality control laboratories
  • Third‑party testing and certification bodies
  • Research labs conducting routine composition analysis of low‑alloy steels
• Typical uses
  • Routine composition verification of unalloyed/low‑alloy steel batches
  • Incoming material inspection, process control and acceptance testing
  • Material certification where accurate Si, Mn, P, Cu, Ni, Cr, Mo, Sn data are required

Related Standards

• EN 10351:2011 - similar ICP‑OES method covering higher chromium levels (up to 1.6 %); EN 10355 is optimised for silicon
• EN ISO 14284 - guidance on sampling of steel materials
• EN ISO 648 / EN ISO 1042 - specifications for laboratory pipettes and volumetric flasks

Keywords: EN 10355:2013, ICP‑OES, inductively coupled plasma optical emission spectrometry, chemical analysis of steels, silicon determination, nitric‑sulphuric digestion, routine method.

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Chemische Analyse von Eisenwerkstoffen - Analyse von unlegierten und niedrig legierten Stähle mittels optischer Emissionsspekrometrie mit indukiv gekoppeltem Plasma - Bestimung von Si, Mn, P, Cu, Ni, Cr, Mo, Sn und Al (lösung) [Routineverfahren]Analyse chimique des matériaux sidérurgiques - Analyse des aciers non alliés et faiblement alliés par spectrométrie d'émission optique avec source à plasma induit - Détermination de Si, Mn, P, Cu, Ni, Cr, Mo, Sn et Al (soluble) [Méthode de routine]Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination of Si, Mn, P, Cu, Ni, Cr, Mo, Sn and Al (soluble) [Routine method]77.080.20JeklaSteels77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 10355:2013SIST EN 10355:2014en,fr,de01-januar-2014SIST EN 10355:2014SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 10355
August 2013 ICS 77.040.30 English Version
Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination of Si, Mn, P, Cu, Ni, Cr, Mo and Sn, following dissolution with nitric and sulphuric acids [Routine method]
Analyse chimique des matériaux ferreux - Analyse des aciers non alliés et faiblement alliés par spectrométrie d'émission optique avec source à plasma induit - Détermination de Si, Mn, P, Cu, Ni, Cr, Mo et Sn, après mise en solution par les acides nitrique et sulfurique [Méthode de routine]
Chemische Analyse von Eisenwerkstoffen - Analyse von unlegierten und niedrig legierten Stählen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma -Bestimmung von Si, Mn, P, Cu, Ni, Cr, Mo und Sn nach Lösen in Salpeter- und Schwefelsäure [Routineverfahren] This European Standard was approved by CEN on 29 June 2013.
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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 10355:2013: ESIST EN 10355:2014

Plasma optical emission spectrometer — Suggested performance criteria to be checked . 18 Annex B (normative)
Synoptic of the operations related to Clause 9 . 22 Annex C (informative)
Composition of the test samples used for the validation precision test . 23 Annex D (informative)
Detailed results obtained from the validation precision test . 24 Annex E (informative)
Graphical representation of the precision data . 32 Bibliography. 39
Table 1 — Application ranges
Element Mass fraction % min. max. Si 0,020 0,45 Mn 0,005 1,40 P 0,005 0,10 Cu 0,005 0,60 Ni 0,010 2,00 Cr 0,010 0,90 Mo 0,005 0,60 Sn 0,010 0,10
NOTE For tin, see NOTE 2 under Clause 11. In all cases, the ranges specified can be extended or adapted (after validation) for the determination of other mass fractions, provided that the iron content in the samples under concern is above 95 %. Other elements may be included. However such elements and their mass fractions should be carefully checked, taking into account the possible interferences, the sensitivity, the resolution and the linearity criteria of each instrument and each wavelength. Depending also on the sensitivity of each instrument, suitable dilutions of the calibration and the test sample solutions may be necessary. Moreover, even if the method described is "multi elemental", it is not absolutely necessary to carry out the determination of all the elements of its scope simultaneously. The measurement conditions have to be optimised by each laboratory, depending on the performances of each apparatus available. 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 648, Laboratory glassware — Single-volume pipettes (ISO 648) EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042) SIST EN 10355:2014

1) Covers made from other materials can be suitable, provided that these materials are free from contamination. SIST EN 10355:2014

Element Label F1 F2 F3 F4 Si (4.16) 0,1 mg [0,02 %] a 0,25 mg [0,05 %] b 2,25 mg [0,45 %] c 0,5 mg [0,1 %] d Mn (4.12) 7 mg [1,4 %] 7 ml 1 mg [0,2 %] 1 ml 0,025 mg [0,005 %] e 0,1 mg [0,02 %] f P (4.15) 0,025 mg [0,005 %] g 0,05 mg [0,01 %] h 0,25 mg [0,05 %] i 0,5 mg [0,1 %] j Cu (4.11) 0,25 mg [0,05 %] k 3,0 mg [0,6 %] 3 ml 0,025 mg [0,005 %] l 0,5 mg [0,1 %] m Ni (4.14) 10 mg [2,0 %] 10 ml 2,5 mg [0,5 %] 2,5 ml 0,05 mg [0,01 %] n 0,25 mg [0,05 %] o Cr (4.10) 0,05 mg [0,01 %] p 0,25 mg [0,05 %] q 4,5 mg [0,9 %] 4,5 ml 2,5 mg [0,5 %] 2,5 ml Mo (4.13) 0,05 mg [0,01 %] r 0,25 mg [0,05 %] s 3 mg [0,6 %] 3 ml 0,5 mg [0,1 %] t Sn (4.17) 0,5 mg [0,1 %] u 0,05 mg [0,01 %] v 0,25 mg [0,05 %] w 0,1 mg [0,02 %] x a
1 ml of a 0,1 g/l silicon standard solution m 5,0 ml of a 0,1 g/l copper standard solution b
2,5 ml of a 0,1 g/l silicon standard solution n 5,0 ml of a 0,01 g/l nickel standard solution c
22,5 ml of a 0,1 g/l silicon standard solution o 2,5 ml of a 0,1 g/l nickel standard solution d
5,0 ml of a 0,1 g/l silicon standard solution p 2,5 ml of a 0,01 g/l chromium standard solution e
2,5 ml of a 0,01 g/l manganese standard solution q 2,5 ml of a 0,1 g/l chromium standard solution f
10 ml of a 0,01 g/l manganese standard solution r
5,0 ml of a 0,01 g/l molybdenum standard solution g
2,5 ml of a 0,01 g/l phosphorus standard solution s
2,5 ml of a 0,1 g/l molybdenum standard solution h
5,0 ml of a 0,01 g/l phosphorus standard solution t
5,0 ml of a 0,1 g/l molybdenum standard solution i
2,5 ml of a 0,1 g/l phosphorus standard solution u
5,0 ml of a 0,1 g/l tin standard solution j
5,0 ml of a 0,1 g/l phosphorus standard solution v
5,0 ml of a 0,01 g/l tin standard solution k
2,5 ml of a 0,1 g/l copper standard solution w 2,5 ml of a 0,1 g/l tin standard solution l
2,5 ml of a 0,01 g/l copper standard solution x
10,0 ml of a 0,01 g/l tin standard solution
8.3 Re-calibration Drifts in the spectrometer readings shall be corrected by using the re-calibration procedure as described in the manufacturer's instruction manual. For that purpose the synthetic multi-elemental solutions (8.2), used for the calibration or suitable Certified Reference Materials or Internal Reference Materials solutions may be used. It is strongly recommended to carry out a re-calibration of the instrument before the analysis of each set of unknown samples. SIST EN 10355:2014

Depending on the instrument configuration these parameters may include the outer, intermediate or central gas flow-rates, the torch position, the entrance slits, the exit slits and the photomultiplier tubes voltage. Other wavelengths may be used, provided that interferences, sensitivity, resolution and linearity criteria have been carefully investigated. Prepare the software for measurements of the intensity, and for the calculation of the mean value and relative standard deviation corresponding to each analytical line. Each time the internal reference element is used, prepare the software to calculate the ratio between the intensity of each analyte and the intensity of the internal reference element. 9.3 Spectrometric measurements of the calibration solutions Carry out the spectrometric measurements of the calibration solutions (8.2). A simultaneous spectrometer shall be available for measurements using the internal reference element (ratio mode). For each calibration solution, three to five integrations are necessary in order to calculate the mean intensities or the mean ratioed intensities. SIST EN 10355:2014
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