EN 10351-2011 en Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination of .pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 10351:2011Chemical analysis of ferrousmaterials Inductivelycoupled plasma opticalemission spectrometric analysisof unalloyed and low alloyedsteels Determination of Mn,P, Cu

2、, Ni, Cr, Mo, V, Co, Al (total)and Sn Routine methodBS EN 10351:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 10351:2011.The UK participation in its preparation was entrusted to TechnicalCommittee ISE/102, Methods of Chemical Analysis for Iron and Steel.A

3、 list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 67712 0ICS 77.080.20; 77.140.10; 77.140.45C

4、ompliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 March 2011.Amendments issued since publicationDate Text affectedBS EN 10351:2011EUROPEAN STANDARD NORME EUROPENNE

5、 EUROPISCHE NORM EN 10351 March 2011 ICS 77.140.10; 77.140.45 English Version Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determination of Mn, P, Cu, Ni, Cr, Mo, V, Co, Al (total) and Sn Routine met

6、hod Analyse chimique des matriaux ferreux - Analyse des aciers non allis et faiblement allis par spectromtrie dmission optique avec source plasma induit - Dtermination de Mn, P, Cu, Ni, Cr, Mo, V, Co, Al (total) et Sn Mthode de routine Chemische Analyse von Eisenwerkstoffen - Analyse von unlegierten

7、 und niedrig legierten Sthlen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma -Bestimmung von Mn, P, Cu, Ni, Cr, Mo, V, Co, Al (gesamt) und Sn Routineverfahren This European Standard was approved by CEN on 15 January 2011. CEN members are bound to comply with the CEN/CENELEC

8、 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 t

9、o 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 offici

10、al 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, Romania, Slova

11、kia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide

12、for CEN national Members. Ref. No. EN 10351:2011: EBS EN 10351:2011EN 10351:2011 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 54 Reagents .55 Apparatus .86 Sampling .87 Sample solution preparation 88 Calibration process .99 Determination 1210 Expression of results . 151

13、1 Precision 1512 Test report . 19Annex A (informative) Plasma optical emission spectrometer Suggested performance criteria to be checked 20Annex B (normative) Synoptic of the operations related to Clause 9 24Annex C (informative) Test samples used for the validation precision test 25Annex D (informa

14、tive) Detailed results obtained from the validation precision test 26Annex E (informative) Graphical representation of the precision data 35Bibliography . 44BS EN 10351:2011EN 10351:2011 (E) 3 Foreword This document (EN 10351:2011) has been prepared by Technical Committee ECISS/TC 102 “Methods of ch

15、emical 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 endorsement, at the latest by September 2011, and conflicting national standards shall be withdrawn

16、at the latest by September 2011. 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 identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, th

17、e national standards organizations 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, Nether

18、lands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. BS EN 10351:2011EN 10351:2011 (E) 4 1 Scope This European Standard specifies an inductively coupled plasma optical emission spectrometry routine method for the analysis of unalloyed and low a

19、lloyed steels, whose iron content shall be at least 95 %. This method is applicable to the elements listed in Table 1 within the ranges shown. Table 1 Application ranges Element Mass fraction % min. max. Mn 0,005 2,00P 0,005 0,05Cu 0,005 0,80 Ni 0,010 2,00Cr 0,010 1,60Mo 0,005 0,80 V 0,002 0,40Co 0,

20、002 0,10Al (total) 0,020 0,30 Sn 0,001 0,10In 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

21、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

22、 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 pe

23、rformances of each apparatus available. NOTE 1 The accuracy of the method is unsatisfactory for phosphorus contents from 0,05 to 0,1 %. NOTE 2 The trueness of the method couldnt be checked for vanadium contents below 0,05 %. NOTE 3 The precision of the method is unsatisfactory for aluminium (total)

24、contents below 0,02 %. 2 Normative references The following referenced documents are indispensable for the application 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. CEN

25、/TR 10345:2008, Guideline for statistical data treatment of inter laboratory tests for validation of analytical methods BS EN 10351:2011EN 10351:2011 (E) 5 EN ISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical composition (ISO 14284:1996) ISO 648, Laborat

26、ory glassware One-mark pipettes ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and res

27、ults Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method 3 Principle Diss

28、olution of a test portion with nitric and hydrochloric acids. Filtration and ignition of the acid insoluble residue. Removal of silica with hydrofluoric acid. Fusion of the residue with a mixture of orthoboric acid and potassium carbonate, dissolution of the melt with acid and addition of this solut

29、ion to the reserved filtrate. 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

30、relevant, 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.

31、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 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 Hydrofluoric acid, HF (20= 1,13 g/ml

32、) WARNING Hydrofluoric acid is extremely irritating and corrosive to skin and mucous membranes producing severe skin burns which are slow to heal. In the case of contact with skin, wash well with water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate, and seek immediate medica

33、l treatment. 4.6 Sulphuric acid, H2SO4(20= 1,84 g/ml) 4.7 Sulphuric acid, solution 1 + 1 BS EN 10351:2011EN 10351:2011 (E) 6 Add 25 ml of sulphuric acid (4.6) to 25 ml of water and allow it to cool. 4.8 Fusion reagent 4.8.1 Fusion mixture Mix one part by mass of orthoboric acid, H3BO3and one part of

34、 potassium carbonate anhydrous, K2CO3. 4.8.2 Fusion mixture, 100 g/l solution In a suitable beaker, dissolve 25 g of the fusion mixture (4.8.1). Heat if necessary. After cooling, transfer the solution quantitatively into a 250 ml one-mark volumetric flask, dilute to the mark with water and mix well.

35、 4.9 Aluminium, 1 g/l standard solution Weigh (0,5 0,001) g of aluminium (99,99 % purity) and transfer into a 400 ml beaker. Add 50 ml of hydrochloric acid solution (4.2) and heat gently until aluminium is completely dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-ma

36、rk volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Al. 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

37、 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. 4.11 Cobalt 1 g/l standard solution Weigh (0,5 0,001) g of cobalt (99,99 % purity) and transfer i

38、nto a 250 ml beaker. Dissolve it in 5 ml of hydrochloric acid (4.1) and 5 ml of nitric acid (4.3). 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

39、 mark with water and mix well. 1 ml of this solution contains 1 mg of Co. 4.12 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, then boil unti

40、l 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 this solution contains 1 mg of Cu. 4.13 Manganese 1 g/l standard solution The manganese used to prepare the solution is

41、 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 (4.6). Shake and after a few seconds, allow the solution to settle and add water. Repeat the water cleaning several times. Remo

42、ve the metallic manganese and rinse with acetone. Dry the metal in an oven at 100 C for 2 minutes 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 solu

43、tion (4.4). Heat gently until the metal is dissolved. After BS EN 10351:2011EN 10351:2011 (E) 7 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. 4.14 Molybdenum 1 g/l standard

44、 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 dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-mark volumet

45、ric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Mo. 4.15 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 d

46、issolved, 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 this solution contains 1 mg of Ni. 4.16 Phosphorus 1 g/l standard solution Weigh (2,197 0,001)

47、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 water and mix well. 1 ml of this solution contains 1 mg of P. 4.17 Tin 1 g/l standard solution fr

48、eshly 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 the mark wit

49、h water and mix well. 1 ml of this solution contains 1 mg of Sn. 4.18 Vanadium 1 g/l standard solution Weigh (0,5 0,001) g of vanadium (99,99 % purity) and transfer into a 250 ml beaker. Dissolve it in 30 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 thi