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

1、BSI Standards PublicationBS EN 10355:2013Chemical analysis of ferrous materials Inductively coupled plasma optical emis-sion 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 met

2、hodBS EN 10355:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 10355:2013. The UK participation in its preparation was entrusted to TechnicalCommittee ISE/102, Methods of Chemical Analysis for Iron and Steel. A list of organizations represented on this comm

3、ittee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2013.Published by BSI Standards Limited 2013ISBN 978 0 580 76588 9 ICS 77.04

4、0.30 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2013.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS EN 10355:2013EUR

5、OPEAN STANDARD NORME EUROPENNE EUROPISCHE 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, follo

6、wing dissolution with nitric and sulphuric acids Routine method Analyse chimique des matriaux ferreux - Analyse des aciers non 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

7、 nitrique et sulfurique Mthode de routine Chemische Analyse von Eisenwerkstoffen - Analyse von unlegierten und niedrig legierten 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 Ro

8、utineverfahren 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 bibliog

9、raphical 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 responsib

10、ility 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 Republi

11、c 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 COMIT EUROPEN DE NORMALIS

12、ATION EUROPISCHES KOMITEE FR 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: EBS EN 10355:2013EN 10355:2013 (E) 2 Contents Page Foreword . 3 1 Scope 4 2

13、Normative references . 4 3 Principle 5 4 Reagents . 5 5 Apparatus . 7 6 Sampling . 7 7 Sample solution preparation . 7 8 Calibration process 9 9 Determination . 11 10 Expression of results . 14 11 Precision . 14 12 Test report 17 Annex A (informative) Plasma optical emission spectrometer Suggested p

14、erformance 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

15、 E (informative) Graphical representation of the precision data . 32 Bibliography 39 BS EN 10355:2013EN 10355:2013 (E) 3 Foreword This document (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

16、 SIS. 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 February 2014, and conflicting national standards shall be withdrawn at the latest by February 2014. Attention is drawn to the possibility tha

17、t some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC 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

18、 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, Ro

19、mania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 10355:2013EN 10355:2013 (E) 4 1 Scope This European Standard specifies an inductively coupled plasma optical emission spectrometry routine method for the analysis of unalloyed and low alloyed steels, whose ir

20、on 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

21、 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 o

22、f 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

23、(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

24、 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

25、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 pa

26、rt, 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 pi

27、pettes (ISO 648) EN ISO 1042, Laboratory glassware One-mark volumetric flasks (ISO 1042) BS EN 10355:2013EN 10355:2013 (E) 5 3 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 hy

28、drogen peroxide solution. After suitable dilution and, if necessary, addition of an internal reference element, nebulisation of the solution into an inductively coupled plasma optical emission spectrometer and measurement of the intensity of the emitted light from each element (including, where rele

29、vant, the intensity of the internal reference element). 4 Reagents During the analysis, use only reagents of recognised analytical 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

30、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 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)

31、. 4.6 Hydrogen peroxide, H2O2 30 % (mass fraction) solution. 4.7 Hydrogen peroxide, H2O23 % (mass fraction) solution. Dilute 50 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 sulphur

32、ic acid (4.5) and mix. After cooling, dilute to 1 l with water and mix. 4.9 Ammonium peroxodisulphate solution, 20 g/l. Dissolve 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 beake

33、r. Add 40 ml of hydrochloric acid (4.1) and heat gently until chromium is completely 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 Cr. BS EN 10355:2013EN 10355

34、: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 ml 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, transfe

35、r 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 Cu. 4.12 Manganese 1 g/l standard solution. The manganese used to prepare the solution is released from superficial oxide possibly present by intr

36、oducing 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 (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

37、 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 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. Aft

38、er 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 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 beak

39、er. Dissolve it in 10 ml of hydrochloric acid (4.1) and 10 ml of nitric acid (4.3). 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 o

40、f 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 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

41、 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 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

42、it with water. 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 P. 4.16 Silicon 1 g/l standard solution. Using a suitable plastic beaker, dissolve (3,171 0,001) g of dried ammonium hexaflu

43、orosilicate (NH4)2SiF6 in hot water ( 80 C). Allow to cool and transfer the solution quantitatively into a polyethylene 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. BS EN 10355:2013EN 10355:2013 (E) 7 1 ml of this solution contains 1 mg of Si. 4.17 Tin 1 g/l standard

44、 solution freshly prepared. Weigh (0,5 0,001) g of tin (99,99 % purity) and transfer into a 250 ml beaker. Dissolve 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

45、 the mark with water and mix well. 1 ml of this solution contains 1 mg of Sn. NOTE Standard solutions whose preparations 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 d

46、ocumented. 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 l

47、ower limit of each element as given in the scope. 5 Apparatus All volumetric glassware shall be class A and calibrated in accordance with EN ISO 648 or EN ISO 1042, as appropriate. 5.1 Microwave system. 5.2 Gravimetric or volumetric dispensers. 5.3 Optical emission spectrometer, equipped with induct

48、ively coupled plasma. This shall be equipped with a nebulisation system. The instrument used will be satisfactory if, after optimising in accordance with the manufacturers instructions, it meets the performance criteria given in Annex A. 6 Sampling Sampling shall be carried out in accordance with EN

49、 ISO 14284 or with an appropriate national standard for steel. 7 Sample solution preparation 7.1 General The method is optimised for use with automated systems, open microwave digestion units (5.1) and gravimetric dispensers (5.2). NOTE This method was also tested with closed microwave units, after a suitable optimisation of the relevant operating conditions: temperatures and times. BS EN 10355:2013EN 10355:2013 (E) 8 The method can also be used in a classical way with hot plates and manual additions. 7.2 Test portion We