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1、BRITISH STANDARD BS EN 10184:1992 Chemical analysis of ferrous materials Determination of phosphorus in steels and irons Spectrophotometric method The European Standard EN 10184:1989 has the status of a British Standard Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 03:49:44 GMT+00:00 2006,
2、Uncontrolled Copy, (c) BSI BS EN 10184:1992 This British Standard, having been prepared under the direction of the Iron and Steel Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 28 February 1992 BSI 11-1999 The following BSI references re
3、late to the work on this standard: Committee reference ISM/18 Draft for comment 84/38264 DC ISBN 0 580 20578 9 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of th
4、e following countries. AustriaOesterreichisches Normungsinstitut BelgiumInstitut belge de normalisation DenmarkDansk Standardiseringsraad FinlandSuomen Standardisoimisliito, r.y. FranceAssociation franaise de normalisation GermanyDeutsches Institut fr Normung e.V. GreeceHellenic Organization for Sta
5、ndardization IcelandTechnological Institute of Iceland IrelandNational Standards Authority of Ireland ItalyEnte Nazionale Italiano di Unificazione LuxembourgInspection du Travail et des Mines NetherlandsNederlands Normalisatie-instituut NorwayNorges Standardiseringsforbund PortugalInstituto Portugus
6、 da Qualidade SpainAsociacin Espaola de Normalizacin y Certificacin SwedenStandardiseringskommissionen i Sverige SwitzerlandAssociation suisse de normalisation United KingdomBritish Standards Institution Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun,
7、 na, Thu Oct 26 03:49:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 10184:1992 BSI 11-1999i Contents Page Cooperating organizationsInside front cover National forewordii Brief history2 Foreword2 Text of EN 101843 National annex NA (informative) Committees responsibleInside back cover Licensed
8、Copy: sheffieldun sheffieldun, na, Thu Oct 26 03:49:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 10184:1992 ii BSI 11-1999 National foreword This British Standard has been prepared under the direction of the Iron and Steel Standards Policy Committee and is the English language version of EN 1
9、0184:1989 “ Chemical analysis of ferrous materials Determination of phosphorus in steels and irons Spectrophotometric method” , published by the European Committee for Standardization (CEN). It incorporates the Corrigendum EN 10184AC:1991. It supersedes BS 6200-3.24.1:1985, which is withdrawn. A fur
10、ther method for the determination of phosphorus in ferrous materials will shortly be published as BS 6200-3.24.2. Full details of other British Standards relating to the chemical analysis of ferrous materials are given in BS 6200-3.0:1991. A British Standard does not purport to include all the neces
11、sary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN
12、 title page, pages 2 to 12, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 03:49:44 GM
13、T+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 10184 May 1989 UDC 669.1:543.422.4:546.18Incorporates Corrigendum September 1991 Descriptors: Iron- and steel products, steels, cast iron, chemical analysis, determination of content, phosphorus, spectropho
14、tometric analysis, phospho-vanado-molybdate, molecular absorption spectrophotometry. English version Chemical analysis of ferrous materials Determination of phosphorus in steels and irons Spectrophotometric method Analyse chimique des matriaux sidrurgiques Dosage du phosphore dans les aciers et font
15、es Mthode spectrophotomtrique Chemische Analyse von Eisenwerkstoffen Bestimmung von Phosphor in Stahlen und Eisen Spektralphotometrisches Verfahren This European Standard was approved by CEN on 1989-05-15. CEN members are bound to comply with the requirements of the CEN/CENELEC Internal Regulations
16、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 Central Secretariat or to any CEN member. This European
17、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 Central Secretariat has the same status as the official versions. CEN members are the national
18、standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung
19、 Central Secretariat: rue de Stassart 36, B-1050 Brussels CEN 1989 Copyright reserved to all CEN members Ref. No. EN 10184:1989 E Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 03:49:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ? ith stipulatetipulat national standnational stan te lists and
20、 bible lists and b dards may be obtas may be o CEN member.EN member. This EuropeThis Europ GermanGerma respre ? e von EisenwEisenw on Phosphor iosphor i Spektralphotoktralphoto approved by Croved by e requiremrequirem e cone co EN 10184:1989 BSI 11-1999 2 Brief history This European Standard takes o
21、ver the contents of EURONORM 184-87 “ Chemical analysis of ferrous materials Determination of phosphorus in steels and irons Spectrophotometric method” prepared by ECISS/TC 20 “ Methods of chemical analysis” , the secretariat of which is allocated to the Dansk Standardiseringsraad (DS). It was submi
22、tted to the CEN Formal Vote following the decision of the Coordinating Commission (COCOR) of the European Committee for Iron and Steel Standardization on 1987-11-24/25. According to the Common CEN/CENELEC Rules, the following countries are bound to implement this European Standard: Austria, Belgium,
23、 Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and United Kingdom. Foreword This European Standard specifies two methods for the spectrophotometric determination of phosphorus. The first method is applicable
24、 to steels and irons and corresponds to International Standard ISO 2732:1984. The second method is applicable to non-alloyed steels and irons. Contents Page Brief history2 Foreword2 Method 1 1Scope and field of application3 2Reference3 3Principle3 4Reagents3 5Apparatus4 6Sampling4 7Procedure4 7.1Tes
25、t portion4 7.2Blank test4 7.3Determination4 7.4Establishment of the calibration graph5 8Expression of results6 9Notes6 10Test report6 Method 2 1Scope and field of application7 2Reference7 3Principle7 4Reagents7 5Apparatus8 6Sampling8 7Procedure8 7.1Test portion8 7.2Blank test8 7.3Determination8 7.4E
26、stablishment of the calibration graph9 8Expression of results10 9Note10 10Test report10 Annex Precision data11 Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 03:49:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ? ons ns rd e to non-alloyed to non-alloye ? alibration graption grap sults report
27、port od 2 1Scope anScope an 2 2RefRe EN 10184:1989 BSI 11-19993 Method 1 Steel and cast iron Determination of phosphorus content Phosphovanadomolybdate spectrophotometric method1) 1 Scope and field of application This European Standard specifies a spectrophotometric method for the determination of p
28、hosphorus in steel and cast iron. The method is applicable to phosphorus contents between 0.005 and 1.5 % (m/m), provided that tungsten, niobium, tantalum and zirconium contents are not higher than 1 % (m/m) for each of these four elements and titanium content is not higher than 2 % (m/m). 2 Referen
29、ce Euronorm 18 Selection and preparation of samples and test pieces for steel and iron and steel products. 3 Principle Dissolution of a test portion in an oxidizing acid mixture. Conversion of phosphorus to phosphovanadomolybdate in perchloric-nitric acid solution. Extraction of phosphovanadomolybda
30、te into 4-methyl-2-pentanone with citric acid present to complex arsenic. Spectrophotometric measurement at a wavelength of about 425 nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity.
31、Verify by blank tests that the relevant reagents are free from phosphorus. Whenever necessary, the results shall be corrected accordingly. Grades giving high blank values are unsuitable and should be discarded. 4.1 Pure iron, containing 0.001 % (m/m) or less of phosphorus. 4.2 Hydrochloric acid, abo
32、ut 1.19 g/ml. 4.3 Nitric acid, about 1.40 g/ml. 4.4 Nitric acid, diluted 1 + 4. 4.5 Perchloric acid, about 1.54 g/ml, with known low phosphorus content. NOTEPerchloric acid ( about 1.67 g/ml) may also be used. 100 ml of perchloric acid ( about 1.54 g/ml) is equivalent to 79 ml of perchloric acid ( a
33、bout 1.67 g/ml). 4.6 Citric acid, solution Dissolve 500 g of citric acid monohydrate (H8C6O7 H2O) in water, dilute to 1 000 ml and mix. 4.7 4-Methyl-2-pentanone (isobutyl methyl ketone). 4.8 Hexaammonium heptamolybdate, solution. Dissolve 15 g of hexaammonium heptamolybdate tetrahydrate (NH4)6Mo7O24
34、 4H2O in water, dilute to 100 ml and mix. 4.9 Ammonium metavanadate, solution. Dissolve 2.5 g of ammonium metavanadate (NH4VO3) in water, dilute to 1 000 ml and mix. 4.10 Boron fluoride, solution. Dissolve 40 g of boric acid (H3BO3) in 300 ml of water in a plastic beaker, add 100 ml of hydrofluoric
35、acid about 1.13 g/ml, dilute to 1 000 ml and mix. Keep the solution in a plastic bottle. 4.11 Potassium permanganate, 10 g/l solution. 4.12 Sodium nitrite, 50 g/l solution. 1)The text of this European Standard corresponds with the text of ISO 2732:1984. Licensed Copy: sheffieldun sheffieldun, na, Th
36、u Oct 26 03:49:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI nt purpu elevant reagevant rea ngly. Grades givinly. Grades giv inin ng g 0.000.001 %1 % (m/m/ ric acidacid, abou abo t 1 c acidacid, , abouabout t 1.41 ric acidic acid, dilute, dilut loric aloric a ? c acid solutionid solution arsenic.rse
37、nic. t 425 5 nm.nm ed, use only reuse only re y. t EN 10184:1989 4 BSI 11-1999 4.13 Phosphorus, standard solution. 4.13.1 Phosphorus, 0.1 g/l stock solution. Weigh, to the nearest 0.0001 g, 0.4393 g of potassium dihydrogen orthophosphate (KH2PO4), previously dried to constant mass at 105 C and coole
38、d in a desiccator. Dissolve in water, transfer quantitatively to a 1 000 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this solution contains 0.1 mg of P. 4.13.2 Phosphorus, 0.01 g/l standard solution. Transfer 100.0 ml of the stock solution (4.13.1) to a 1 000 ml one-mark volume
39、tric flask, dilute to the mark with water and mix. This solution should be prepared immediately before use. 1 ml of this solution contains 0.01 mg of P. 5 Apparatus Ordinary laboratory apparatus and spectrophotometer. 6 Sampling Carry out sampling in accordance with Euronorm 18. 7 Procedure WARNING:
40、 Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or organic material in general. 7.1 Test portion Weigh, to the nearest 0.001 g, approximately 0.5 g (m) of the test sample. 7.2 Blank test In parallel with the determination and following the same procedure, carry
41、 out a blank test using the same quantities of all the reagents. 7.3 Determination 7.3.1 Preparation of test solution 7.3.1.1 For phosphorus content equal to or less than 0.08 % (m/m) Introduce the test portion (7.1) into a 125 ml conical beaker. Add 5 ml of the nitric acid (4.3) and 5 ml of the hyd
42、rochloric acid (4.2), cover the beaker with a watch-glass and heat until solvent action ceases (see Note below). Add 10 ml of the perchloric acid (4.5) and evaporate to fuming. Continue fuming for 5 to 10 minutes at such a temperature that a steady reflux of white perchloric acid fumes on the walls
43、of the beaker is maintained (see 9.1). Cool, add 25 ml of the nitric acid (4.4) and a few glass beads and then boil for 1 to 2 minutes (see 9.2). Add 5 ml of the potassium permanganate solution (4.11), boil for 2 minutes, then add 10 ml of the sodium nitrite solution (4.12) and boil until free of ni
44、trous fumes. NOTEFor highly alloyed samples which do not dissolve readily in this acid mixture, further 5 ml additions of the hydrochloric acid (4.2) may be made up to a maximum of 20 ml. 7.3.1.2 For phosphorus content greater than 0.08 % (m/m) Carry out the same procedure as specified in the first
45、paragraph of 7.3.1.1. Dilute to about 100 ml with water, and filter if necessary to remove graphite. Cool, transfer quantitatively into a 200 ml one-mark volumetric flask, dilute to the mark and mix. Take a suitable volume (V) of the solution, containing not more than 0.4 mg of phosphorus. Proceed a
46、s specified in 7.3.1.1 from the second paragraph beginning at “ Add 10 ml of the perchloric acid (4.5) .” to the end of 7.3.1.1. Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 03:49:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ? 0. .5 g5 g (m n and following then and following t s. n of tes
47、t solutioof test solut rus conteus co ? e presence of amesence of am of the tof the EN 10184:1989 BSI 11-19995 7.3.2 Colour development Cool to about 20 C. Add 10.0 ml of the ammonium metavanadate solution (4.9) and 15.0 ml of the hexaammonium heptamolybdate solution (4.8) and then allow to stand at
48、 a temperature between 18 and 25 C for a minimum of 7 minutes. Transfer the solution to a 250 ml separating funnel marked at 100 ml, dilute to the mark with water and mix. Add 10 ml of the citric acid solution (4.6), mix and immediately add 40.0 ml of the 4-methyl-2-pentanone (4.7), and shake the fu
49、nnel for 30 seconds. Allow the two layers to separate and discard the lower (aqueous) layer. Dry the inside of the stem of the separating funnel with a small piece of filter paper. Filter the 4-methyl-2-pentanone layer through a dry rapid paper into a small dry beaker. 7.3.3 Spectrophotometric measurement Carry out the spectrophotometric measurements at 20 1 C in cells of 2 cm optical path at a wavelength of about 425 nm after having adju