DIN EN 10351-2011 en 5525 Chemical analysis of ferrous materials - Inductively coupled plasma optical emission spectrometric analysis of unalloyed and low alloyed steels - Determin.pdf

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1、May 2011 Translation by DIN-Sprachendienst.English price group 17No 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).ICS 77

2、.140.10; 77.140.45!$p_g“1776068www.din.deDDIN EN 10351Chemical analysis of ferrous materials Inductively coupled plasma optical emission spectrometric analysis ofunalloyed and low alloyed steels Determination of Mn, P, Cu, Ni, Cr, Mo, V, Co, Al (total) and Sn RoutinemethodEnglish translation of DIN

3、EN 10351:2011-05Chemische Analyse von Eisenwerkstoffen Analyse von unlegierten und niedrig legierten Sthlen mittels optischerEmissionsspektrometrie mit induktiv gekoppeltem Plasma Bestimmung von Mn, P, Cu, Ni, Cr, Mo, V, Co, Al (gesamt) und Sn RoutineverfahrenEnglische bersetzung von DIN EN 10351:20

4、11-05Analyse chimique des matriaux ferreux Analyse des aciers non allis et faiblement allis par spectromtrie dmission optiqueavec source plasma induit Dtermination de Mn, P, Cu, Ni, Cr, Mo, V, Co, Al (total) et Sn Mthode de routineTraduction anglaise de DIN EN 10351:2011-05www.beuth.deDocument compr

5、ises pagesIn case of doubt, the German-language original shall be considered authoritative.4604.11 DIN EN 10351:2011-05 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ECISS/TC 102 “Methods of chemical analysis for iron and steel” (Secr

6、etariat: SIS, Sweden). The responsible German body involved in its preparation was the 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. 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISC

7、HE 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 method Analy

8、se 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 und nied

9、rig 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 Internal

10、 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

11、 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 versio

12、ns. 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, Slovakia, Slov

13、enia, 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 for CEN n

14、ational Members. Ref. No. EN 10351:2011: EEN 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 . 1511 Precision 1512 Test rep

15、ort . 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 (informative) Detailed results ob

16、tained from the validation precision test 26Annex E (informative) Graphical representation of the precision data 35Bibliography . 44DIN EN 10351:2011-05 EN 10351:2011 (E) 3 Foreword This document (EN 10351:2011) has been prepared by Technical Committee ECISS/TC 102 “Methods of chemical analysis for

17、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 at the latest by Sep

18、tember 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, the national standards

19、 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, Netherlands, Norway, Polan

20、d, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DIN EN 10351:2011-05 EN 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 alloyed steels,

21、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 0,002 0,10Al (tot

22、al) 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 and their mass

23、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 so

24、lutions 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 e

25、ach 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) contents below

26、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/TR 10345:2008,

27、 Guideline for statistical data treatment of inter laboratory tests for validation of analytical methods DIN EN 10351:2011-05 EN 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, Laboratory glassw

28、are 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 results Part

29、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 Dissolution of

30、 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 solution to the

31、 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 relevant,

32、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 Hydroc

33、hloric 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) WARNING

34、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 medical treatmen

35、t. 4.6 Sulphuric acid, H2SO4(20= 1,84 g/ml) 4.7 Sulphuric acid, solution 1 + 1 DIN EN 10351:2011-05 EN 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 pota

36、ssium 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. 4.9

37、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-mark vo

38、lumetric 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 comp

39、letely 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 into a

40、 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 mark

41、 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 until nit

42、rous 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 rele

43、ased 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. Remove th

44、e 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 solution

45、(4.4). Heat gently until the metal is dissolved. After DIN EN 10351:2011-05 EN 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

46、 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

47、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

48、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)

49、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 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