DIN EN 10184-2006 Chemical analysis of ferrous materials - Determination of phosphorus in non-alloyed steels and irons - Molybdenum blue spectrophotometric method English version o.pdf

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1、 DEUTSCHE NORMMay 2006DIN EN 10184 ICS 77.040.30 Supersedes DIN EN 10184:1990-04 Chemical analysis of ferrous materials Determination of phosphorus in non-alloyed steels and irons Molybdenum blue spectrophotometric method; English version of DIN EN 10184:2006-05 Chemische Analyse von Eisenwerkstoffe

2、n Bestimmung von Phosphor in unlegierten Sthlen und Eisen Spektralphotometrisches Verfahren ber Molybdnblau; Englische Fassung DIN EN 10184:2006-05 Document comprises 13 pages No part of this standard may be reproduced without prior permission of DIN Deutsches Institut fr Normung e. V., Berlin. Beut

3、h Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). English price group 8 www.din.de www.beuth.de !,nle“10.06 9757366DIN EN 10184:2006-05 2 National foreword This standard has been prepared by ECISS/TC 20 Methods of chemical analysis of ferrous pr

4、oducts (Secretariat: Sweden). The responsible German body involved in its preparation was the Normenausschuss Eisen und Stahl (Steel and Iron Standards Committee), Technical Committee 30 Analyseverfahren. This European Standard specifies a method of determining phosphorous in non-alloyed steels and

5、iron by molybdenum blue spectrophotometry. Amendments This standard differs from DIN EN 10184:1990-04 as follows: a) Since method 1 has been deleted, the former method 2 is now the standard method. b) As a result of the deletion of method 1, the scope has been confined to phosphorous contents up to

6、0,25 % (m/m). c) The standard has been editorially revised. Previous edition DIN EN 10184:1990-04 EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 10184February 2006ICS 77.040.30 Supersedes EN 10184:1989 English VersionChemical analysis of ferrous materials - Determination ofphosphorus in non-alloy

7、ed steels and irons - Molybdenum bluespectrophotometric methodAnalyse chimique des matriaux sidrurgiques -Dtermination du phosphore dans les aciers et fontes nonallis - Mthode par spectrophotomtrie au bleu demolybdneChemische Analyse von Eisenwerkstoffen - Bestimmungvon Phosphor in unlegierten Sthle

8、n und Eisen -Spektralphotometrisches Verfahren ber MolybdnblauThis European Standard was approved by CEN on 30 December 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard wit

9、hout any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language ma

10、de by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Gr

11、eece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement

12、Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 10184:2006: EEN 10184:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents.4 5 Apparatus .6 6 S

13、ampling.6 7 Procedure .6 8 Expression of results 8 9 Note .9 10 Test report 9 Annex A (informative) Precision data10 Bibliography 11 EN 10184:2006 (E) 3 Foreword This European Standard (EN 10184:2006) has been prepared by Technical Committee ECISS/TC 20 “Methods of chemical analysis of ferrous produ

14、cts”, 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 August 2006, and conflicting national standards shall be withdrawn at the latest by August 2006. This

15、 European Standard supersedes EN 10184:1989. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece,

16、 Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 10184:2006 (E) 4 1 Scope This European Standard specifies a method for the molybdenum blue spectrophotometric

17、 determination of phosphorus in non-alloyed steels and irons. The method is applicable to non-alloyed steels and irons with phosphorus contents from 0,005 % to 0,25 % (m/m). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated re

18、ferences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical composition (ISO 14284:1996) 3 Principle Dissolution

19、of a test portion in nitric and hydrochloric acids and controlled addition of perchloric acid. Formation of the phosphomolybdate complex after removal of silicon and arsenic and reduction with hydrazine sulphate to molybdenum blue. Spectrophotometric measurement of the blue complex at a wavelength o

20、f 680 nm or 825 nm. 4 Reagents 4.1 General During the analysis, unless otherwise stated, only reagents of recognized analytical grade shall be used and only distilled water or water of equivalent purity. Blank tests shall verify that the relevant reagents are free from phosphorus. Whenever necessary

21、, the results shall be corrected accordingly. Grades giving high blank values are unsuitable and should be discarded. 4.2 Hydrochloric acid about 1,19 g/ml. 4.3 Nitric acid about 1,40 g/ml. 4.4 Perchloric acid about 1,67 g/ml. EN 10184:2006 (E) 5 4.5 Hydrofluoric acid about 1,13 g/ml, diluted 1 + 9.

22、 4.6 Hydrobromic acid about 1,47 g/ml, diluted 1 + 1. 4.7 Perchloric acid about 1,67 g/ml, diluted 42 + 58. 420 ml perchloric acid (4.4) shall be carefully poured into 400 ml of water. Swirl, cool, transfer to a 1000 ml volumetric flask. Dilute to the mark with water and mix. 4.8 Sulphuric acid abou

23、t 1,84 g/ml, diluted 3 + 37. 37,5 ml sulphuric acid ( about 1,84 g/ml) shall be carefully poured into 300 ml water. Swirl, cool and transfer to a 500 ml volumetric flask. Dilute to the mark with water and mix. 4.9 Sodium metabisulphite 100 g/l solution. 100 g of dry sodium metabisulphite (Na2S2O5) s

24、hall be dissolved in 500 ml of warm water, filter and collect the filtrate in a 1000 ml volumetric flask. Cool, dilute to the mark with water and mix. 4.10 Hydrazine sulphate 1,5 g/l solution to be prepared immediately before use. 4.11 Ammonium molybdate 20 g/l solution. Dissolve 20 g of ammonium mo

25、lybdate (NH4)6Mo7O244H2O in about 100 ml of diluted sulphuric acid (4.8). Dilute to around 500 ml with water. Carefully pour 300 ml of sulphuric acid (4.8) into this solution. Swirl, cool and transfer to a 1000 ml volumetric flask. Dilute to the mark with water and mix. 4.12 Molybdate reagent Prepar

26、e immediately before use the following mixture: Add, in order, to a 1000 ml volumetric flask, swirling between additions: 500 ml of water; 250 ml of molybdate solution (4.11); 100 ml of hydrazine sulphate solution (4.10). Dilute to the mark with water and mix. EN 10184:2006 (E) 6 4.13 Phosphorus 5 m

27、g/l standard solution. Weigh, to the nearest 0,0001 g, 0,4393 g of potassium dihydrogen phosphate (KH2PO4), previously dried to constant mass at 105 C and cooled in a desiccator. Dissolve in water and add 40 ml perchloric acid, about 1,67 g/ml, diluted 1 + 5. Transfer to 1000 ml volumetric flask, di

28、lute to the mark with water and mix. Transfer 50,0 ml of this solution to a 1000 ml volumetric flask, dilute to the mark with water and mix. 1 ml of this solution contains 5 g of phosphorus. 5 Apparatus Ordinary laboratory equipment and spectrophotometer, suitable for measuring the absorbance of the

29、 solution at a wavelength of 680 nm or 825 nm, together with 2 cm or 1 cm optical cells. 6 Sampling Sampling shall be carried out in accordance with EN ISO 14284. Chips of thickness less than 2 mm. 7 Procedure 7.1 Test portion Weigh a mass (m) to the nearest 0,001 g: m = 1 g 5 % for 0,005 1 %), repe

30、at the step given in the second paragraph of 7.3.1 as often as necessary for the complete removal of silicon. 10 Test report The test report shall include the following information: a) method used by reference to this European Standard; b) results, and the form in which they are expressed; c) any un

31、usual features noted during the determination; d) any operation not specified in this European Standard or in the European Standard to which reference is made, or any optional operation which may have influenced the results. EN 10184:2006 (E) 10 Annex A (informative) Precision data Planned trials of

32、 this method were carried out by analysts from 15 laboratories; each analyst carried out two determinations on each of five samples. From the results obtained 95 % (2 s) confidence limits have been calculated in accordance with ISO 5725 and are tabulated as follows: Table A.1 Precision data Alloy ty

33、pe Content of phosphorus% Repeatability r Reproducibility R Non-alloyed irona Non-alloyed steel Non-alloyed steel Non-alloyed steel Non-alloyed steel 0,02 0,02 0,024 0,043 0,012 0,0013 0,0014 0,0019 0,0027 0,0024 0,0023 0,0019 0,0028 0,0041 0,0030 aIn the case of this iron, only five laboratories pa

34、rticipated in the tests. Repeatability, r The difference between two single results found on identical material by one analyst using the same apparatus within a short time interval will exceed the repeatability, r, on average not more than once in 20 cases in the normal and correct operation of the

35、method. Reproducibility, R The difference between two single and independent results found by two operators working in different laboratories on identical test material will exceed the reproducibility, R, on average not more than once in 20 cases in the normal and correct operation of the method. EN

36、 10184:2006 (E) 11 Bibliography 1 ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions 2 ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of rep

37、eatability and reproducibility of a standard measurement method 3 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 4 ISO 5725-4:1994, Accuracy (trueness and precision) of measurement

38、methods and results Part 4: Basic methods for the determination of the trueness of a standard measurement method 5 ISO 5725-5:1998, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the determination of the precision of a standard measurement method 6 ISO 5725-6:1994, Accuracy (trueness and precision) of measurement methods and results Part 6: Use in practice of accuracy values