BS EN 10184-2006 Chemical analysis of ferrous materials - Determination of phosphorus in non-alloyed steels and irons - Molybdenum blue spectrophotometric method《黑色金属材料化学分析 非合金钢铁中磷.pdf

1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58of phosphorus in non-alloyed steels and irons Molybdenum blue spectrophotometric methodThe European

2、 Standard EN 10184:2006 has the status of a British StandardICS 77.040.30Chemical analysis of ferrous materials Determination BRITISH STANDARDBS EN10184:2006BS EN 10184:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2006 BSI 2006I

3、SBN 0 580 48271 5Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electro

4、nic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations.Summary of pagesThis d

5、ocument comprises a front cover, an inside front cover, the EN title page, pages 2 to 11 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsA list of organizations represented on th

6、is committee can be obtained on request to its secretary. present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Na

7、tional forewordThis British Standard is the official English language version of EN 10184:2006. It supersedes BS EN 10184:1992 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee ISE/18, Sampling and analysis of iron and steel, which has the responsibilit

8、y to: aid enquirers to understand the text;EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 10184February 2006ICS 77.040.30 Supersedes EN 10184:1989 English VersionChemical analysis of ferrous materials - Determination ofphosphorus in non-alloyed steels and irons - Molybdenum bluespectrophotometric

9、 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 Sthlen und Eisen -Spektralphotometrisches Verfahren ber Moly

10、bdnblauThis 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 without any alteration. Up-to-date lists and bibliographic

11、al 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 made by translationunder the responsibility of a CEN memb

12、er 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, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuan

13、ia, 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 Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN Al

14、l 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 Sampling.6 7 Procedure .6 8 Expression of results 8 9 No

15、te .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 products”, the secretariat of which is held by SIS. This Eur

16、opean 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 European Standard supersedes EN 10184:1989. According

17、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, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, L

18、uxembourg, 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 determination of phosphorus in non-alloyed steels and

19、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 references, only the edition cited applies. For undated r

20、eferences, 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 of a test portion in nitric and hydrochloric acids and

21、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 of 680 nm or 825 nm. 4 Reagents 4.1 General During the a

22、nalysis, 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, the results shall be corrected accordingly. Grades gi

23、ving 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. 4.6 Hydrobromic acid about 1,47 g/ml, diluted 1 + 1. 4

24、.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 about 1,84 g/ml, diluted 3 + 37. 37,5 ml sulphuric acid ( a

25、bout 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) shall be dissolved in 500 ml of warm water, filter and c

26、ollect 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 molybdate (NH4)6Mo7O244H2O in about 100 ml of diluted sul

27、phuric 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 Prepare immediately before use the following mixture: Add, in

28、 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 mg/l standard solution. Weigh, to the nearest 0,0001 g,

29、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, dilute to the mark with water and mix. Transfer 50,0 ml o

30、f 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 solution at a wavelength of 680 nm or 825 nm, together

31、 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 %), repeat the step given in the second paragraph of 7.3.1 as o

32、ften 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 unusual features noted during the determination; d) any o

33、peration 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 this method were carried out by analysts from 15 labor

34、atories; 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 type Content of phosphorus% Repeatability r Reproducibili

35、ty 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 participated in the tests. Repeatability, r The differenc

36、e 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 method. Reproducibility, R The difference between two s

37、ingle 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 10184:2006 (E) 11 Bibliography 1 ISO 5725-1:1994, Accu

38、racy (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 repeatability and reproducibility of a standard measuremen

39、t 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 methods and results Part 4: Basic methods for the deter

40、mination 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) o

41、f measurement methods and results Part 6: Use in practice of accuracy values BS ENBSI389 Chiswick High RoadLondonW4 4AL10184:2006BSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at th

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