DIN EN 10355-2013 Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination ofn.pdf

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1、November 2013 Translation by DIN-Sprachendienst.English price group 16No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).I

2、CS 77.040.30!%*,g“2070968www.din.deDDIN EN 10355Chemical analysis of ferrous materials Inductively coupled plasma optical emission spectrometric analysis ofunalloyed and low alloyed steels Determination of Si, Mn, P, Cu, Ni, Cr, Mo and Sn, following dissolutionwith nitric and sulphuric acids Routine

3、 method;English version EN 10355:2013,English translation of DIN EN 10355:2013-11Chemische Analyse von Eisenwerkstoffen Analyse von unlegierten und niedrig legierten Sthlen mittels optischerEmissionsspektrometrie mit induktiv gekoppeltem Plasma Bestimmung von Si, Mn, P, Cu, Ni, Cr, Mo und Sn nach Ls

4、en in Salpeter- undSchwefelsure Routineverfahren;Englische Fassung EN 10355:2013,Englische bersetzung von DIN EN 10355:2013-11Analyse chimique des matriaux ferreux Analyse des aciers non allis et faiblement allis par spectromtrie dmission optiqueavec source plasma induit Dtermination de Si, Mn, P, C

5、u, Ni, Cr, Mo et Sn, aprs mise en solution par les acidesnitrique et sulfurique Mthode de routine;Version anglaise EN 10355:2013,Traduction anglaise de DIN EN 10355:2013-11www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 41 pages 10.13 D

6、IN EN 10355:2013-11 2 A comma is used as the decimal marker. National foreword This document (EN 10355:2013) has been prepared by Technical Committee CEN/TC 102 “Methods of chemical analysis for iron and steel” (Secretariat: SIS, Sweden). The responsible German body involved in its preparation was t

7、he Normenausschuss Eisen und Stahl (Iron and Steel Standards Committee), Working Committee NA 021-00-30 AA Analysenverfahren. There is no national standard on the subject. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 10355 August 2013 ICS 77.040.30 English Version Chemical analysis of ferrou

8、s 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 matriaux ferreux - Analyse des aciers no

9、n allis et faiblement allis par spectromtrie dmission optique avec source plasma induit - Dtermination de Si, Mn, P, Cu, Ni, Cr, Mo et Sn, aprs mise en solution par les acides nitrique et sulfurique Mthode de routine Chemische Analyse von Eisenwerkstoffen - Analyse von unlegierten und niedrig legier

10、ten Sthlen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma -Bestimmung von Si, Mn, P, Cu, Ni, Cr, Mo und Sn nach Lsen in Salpeter- und Schwefelsure Routineverfahren This European Standard was approved by CEN on 29 June 2013. CEN members are bound to comply with the CEN/CENEL

11、EC 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

12、 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 offi

13、cial 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,

14、 Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation

15、 in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 10355:2013: EEN 10355:2013 (E) 2 Contents Page Foreword . 3 1 Scope 4 2 Normative references . 4 3 Principle 5 4 Reagents . 5 5 Apparatus . 7 6 Sampling . 7 7 Sample solution preparation . 7 8 Calibration process

16、9 9 Determination . 11 10 Expression of results . 14 11 Precision . 14 12 Test report 17 Annex A (informative) 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) Composit

17、ion 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 DIN EN 10355:2013-11 EN 10355:2013 (E) 3 Foreword This d

18、ocument (EN 10355:2013) has been prepared by Technical Committee ECISS/TC 102 “Methods of chemical analysis for iron and steel”, the secretariat of which is held by SIS. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsem

19、ent, at the latest by February 2014, and conflicting national standards shall be withdrawn at the latest by February 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identi

20、fying 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 Yugosl

21、av 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 the United Kingdom. DIN EN 10355:2013-11 EN 10355:2013 (E) 4 1 Scope T

22、his 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 de

23、termination 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

24、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,

25、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 ab

26、ove 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 o

27、f 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 conditi

28、ons 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 c

29、ited 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) DIN EN 10355:2013-11 EN 10355:2013 (E) 5 3

30、 Principle Dissolution of a test portion with a nitric-sulphuric acids mixture. Addition of an ammonium peroxodisulphate solution and boiling. After cooling, addition of a hydrogen peroxide solution. After suitable dilution and, if necessary, addition of an internal reference element, nebulisation o

31、f the solution into an inductively coupled plasma optical emission spectrometer and measurement of the intensity of the emitted light from each element (including, where relevant, the intensity of the internal reference element). 4 Reagents During the analysis, use only reagents of recognised analyt

32、ical grade and only distilled water or water of equivalent purity. The same reagents should be used for the preparation of calibration solutions and of sample solutions. 4.1 Hydrochloric acid, HCl (20= 1,19 g/ml). 4.2 Hydrochloric acid, solution 1 + 1. Add 500 ml of hydrochloric acid (4.1) to 500 ml

33、 of water. 4.3 Nitric acid, HNO3(20= 1,33 g/ml). 4.4 Nitric acid, solution 1 + 1. Add 500 ml of nitric acid (4.3) to 500 ml of water. 4.5 Sulphuric acid, H2SO4(20= 1,84 g/ml). 4.6 Hydrogen peroxide, H2O2 30 % (mass fraction) solution. 4.7 Hydrogen peroxide, H2O23 % (mass fraction) solution. Dilute 5

34、0 ml of hydrogen peroxide (4.6) with water to 500 ml. 4.8 Nitric-sulphuric acids mixture. Add to approximately 500 ml of water 50 ml of nitric acid (4.3) and 50 ml of sulphuric acid (4.5) and mix. After cooling, dilute to 1 l with water and mix. 4.9 Ammonium peroxodisulphate solution, 20 g/l. Dissol

35、ve 10 g of ammonium peroxodisulphate in 500 ml water. 4.10 Chromium 1 g/l standard solution. Weigh (0,5 0,001) g of chromium (99,99 % purity) and transfer into a 250 ml beaker. Add 40 ml of hydrochloric acid (4.1) and heat gently until chromium is completely dissolved. After cooling, transfer the so

36、lution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Cr. DIN EN 10355:2013-11 EN 10355:2013 (E) 6 4.11 Copper 1 g/l standard solution. Weigh (0,5 0,001) g of copper (99,99 % purity) and transfer into a 250 m

37、l beaker. Dissolve it in 10 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved and then boil until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml o

38、f this solution contains 1 mg of Cu. 4.12 Manganese 1 g/l standard solution. The manganese used to prepare the solution is released from superficial oxide possibly present by introducing a few grams of metal in a 250 ml beaker containing (150 to 160) ml of water and (15 to 20) ml of sulphuric acid (

39、4.5). Shake and after a few seconds, allow the solution to settle and add water. Repeat the water cleaning several times. Remove the metallic manganese and rinse with acetone. Dry the metal in an oven at 100 C for 2 min or with a hair dryer. Cool in a desiccator. Weigh (0,5 0,001) g of this purified

40、 manganese and transfer into a 250 ml beaker. Dissolve it in 5 ml of hydrochloric acid (4.1) and 10 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water a

41、nd mix well. 1 ml of this solution contains 1 mg of Mn. 4.13 Molybdenum 1 g/l standard solution. Weigh (0,5 0,001) g of molybdenum (99,99 % purity) and transfer into a 250 ml beaker. Dissolve it in 10 ml of hydrochloric acid (4.1) and 10 ml of nitric acid (4.3). Heat gently until the metal is dissol

42、ved. After cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Mo. 4.14 Nickel 1 g/l standard solution. Weigh (0,5 0,001) g of nickel (99,99 % purity) and transfer into a 250 ml beak

43、er. Dissolve it in 10 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, and then boil until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of thi

44、s solution contains 1 mg of Ni. 4.15 Phosphorus 1 g/l standard solution. Weigh (2,197 0,001) g of dried potassium dihydrogen phosphate, transfer into a 250 ml beaker and dissolve it with water. Transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with wate

45、r and mix well. 1 ml of this solution contains 1 mg of P. 4.16 Silicon 1 g/l standard solution. Using a suitable plastic beaker, dissolve (3,171 0,001) g of dried ammonium hexafluorosilicate (NH4)2SiF6 in hot water ( 80 C). Allow to cool and transfer the solution quantitatively into a polyethylene 5

46、00 ml one-mark volumetric flask, dilute to the mark with water and mix well. DIN EN 10355:2013-11 EN 10355:2013 (E) 7 1 ml of this solution contains 1 mg of Si. 4.17 Tin 1 g/l standard solution freshly prepared. Weigh (0,5 0,001) g of tin (99,99 % purity) and transfer into a 250 ml beaker. Dissolve

47、it in 50 ml of hydrochloric acid (4.1). Heat gently until the metal is dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Sn. NOTE Standard solutions whose preparat

48、ions are described in 4.10 to 4.17 can be replaced by commercially available standard solutions, provided that they are supplied by a recognised producer and their traceability fully documented. 4.18 Internal reference element solution, 1 g/l. Choose a suitable element to be added as internal reference and prepare a 1 g/l solution. NOTE Elements such as Sc and Y are often used for this purpose. 4.19 Pure iron. The iron selected shall have a content of less than one tenth of the lo