1、BRITISH STANDARD BS EN ISO 13900:2002 Steel Determination of boron content Curcumin spectrophotometric method after distillation The European Standard EN ISO 13900:2002 has the status of a British Standard ICS 77.080.20 BS EN ISO 13900:2002 This British Standard, having been prepared under the direc
2、tion of the Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 2 August 2002 BSI 2 August 2002 ISBN 0 580 40172 3 National foreword This British Standard is the official English language version of EN ISO 13900:2002.
3、It is identical with ISO 13900:1997. It supersedes BS 6200-3.5.3:1998 which is withdrawn.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 responsibility to: A list of organizations represented on this committ
4、ee can be obtained on request to its secretary. Cross-references The 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 “Sea
5、rch” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal
6、 obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Sum
7、mary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, page ii, pages 1 to 11, the Annex ZA page, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the docu
8、ment was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO13900 July2002 ICS77.080.20 Englishversion SteelDeterminationofboroncontentCurcumin spectrophotometricmethodafterdistillation(ISO13900:1997) AciersDosageduboreMthodespe
9、ctrophotomtrique lacurcumineaprsdistillation(ISO13900:1997) StahlBestimmungdesBorgehaltesCurcuminVerfahren FotometrischeBestimmungnachDestillation(ISO 13900:1997) ThisEuropeanStandardwasapprovedbyCENon26May2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditio
10、nsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversi
11、oninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxe
12、mbourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENn
13、ationalMembers. Ref.No.ENISO13900:2002EINESO31:0092002(E) 2 Foreword ThetextoftheInternationalStandardfromTechnicalCommitteeISO/TC17“Steel“ofthe InternationalOrganizationforStandardization(ISO)hasbeentakenoverasaEuropean StandardbyTechnicalCommitteeECISS/TC20“Methodsofchemicalanalysisofferrous produ
14、cts“,thesecretariatofwhichisheldbySIS. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbyJanuary2003,andconflictingnati onal standardsshallbewithdrawnatthelatestbyJanuary2003. AccordingtotheCEN/CENELECInternalRegulations,th
15、enationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,Switzerlandandthe UnitedKingdom. Endorsementnotice Thet
16、extoftheInternationalStandardISO13900:1997hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO13900:2002INTERNATIONAL STANDARD IS0 13900 First edition 1997-08- 15 Steel - Determination of boron content -
17、Curcumin spectrophotometric method after distillation Aciers - Dosage du bore - Mhc=c ;ten004=a ;osi=p ;scosi=o lartnec=s detnirP ni dnalreztiwS ii ENISO13900:2002iiLANOITANRETNI DRADNATS o 0SI (7991:00931OSI )E Steel - Determination of boron content - Curcumin spectrophotometric method after distil
18、lation 1 scope This International Standard specifies a method for the determination of the boron content in steel using a curcumin spectrophotometric method after distillation. The method is applicable to a boron content of between 0,000 05 % (m/m) and 0,001 0 % (m/m). 2 Normative references The fol
19、lowing standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are en
20、couraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 385-l :I 984, Laboratory glassware - Burettes - Part 1: General requirements. IS0 648: 1977, Labora
21、tory glassware - One-mark pipettes. IS0 1042: -I), Laboratory glassware - One-mark volumetric flasks. IS0 3696:1987, Water for analytical laboratory use - Specification and test methods. IS0 5725-l :I 994, Accuracy (trueness and precision) of measurement methods and results - Par? I: General princip
22、les and definitions. IS0 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 measurement method. IS0 5725-3:1994, Accuracy (trueness and precision) of measurement methods and
23、 results - Pat? 3: Intermediate measures of the precision of a standard measurement method. IS0 14284 :I 996, Steel and iron - Sampling and preparation of samples for the determination of chemical composition. 3 Principle Dissolution of a test portion in hydrochloric and nitric acids. 1) To be publi
24、shed. (Revision of IS0 1042:1983) 1 ENISO13900:200210SI :00931 )E(7991 0 0SI Decomposition of boron compounds (nitrides etc.) with orthophosphoric and sulfuric acids at a temperature of 290 OC. Distillation of the solution after the addition of methanol and collection of methylborate in a receiver c
25、ontaining sodium hydroxide solution. Evaporation of the solution to dryness. methanol medium. Formation of a coloured complex between orthoboric acid and curcumin in a Spectrophotometric measurement at a wavelength of about 550 nm. 4 Reagents During the analysis, unless otherwise stated, use only re
26、agents of recognized analytical grade and only grade 2 water as specified in IS0 3696. 4.1 Pure iron, free from boron or with a known residual amount of boron. 4.2 Hydrochloric acid, p about 1,19 g/ml. 4.3 Nitric acid, p about 1,40 g/ml. 4.4 Sulfuric acid, p about 1,84 g/ml. 4.5 Orthophosphoric acid
27、, p about 1,71 g/ml, boron content less than 0,02 pg/ml. 4.6 Acetic acid, free from aldehyde, p about 1,05 g/ml. In order to test the acetic acid for the presence of aldehyde, pour 20 ml of acetic acid (p about I,05 g/ml) and 1 ml of potassium permanganate solution (1 g/l) into a 50 ml beaker. In th
28、e absence of aldehyde, the initial violet colour of potassium permanganate will persist ; otherwise the solution will become an easily identifiable brown colour after 15 min. 4.7 Acid mixture A Add one volume of hydrochloric acid (4.2) to two volumes of acetic acid (4.6). 4.8 Acid mixture B While co
29、oling under water and swirling, add in small portions a volume of sulfuric acid (4.4) to an equal volume of acetic acid (4.6). 4.9 Sodium hydroxide, 8 g/l solution. 4.10 Methanol, minimum assay 99,6 % (VW). 4.11 Boron, standard solution. 4.11 .l Stock solution, corresponding to 0,lO g of boron per l
30、itre. Weigh, to the nearest 0,000 1 g, 0,286 0 g of orthoboric acid (H,BO,). Place in a 250 ml beaker and dissolve in about 200 ml of water. Transfer the solution quantitatively to a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. Store in a polypropylene bottle (5.2). 1 ml
31、of this stock solution contains 0,lO mg of boron. ENISO13900:200220 0SI 0SI :00931 )E(7991 4.11.2 Standard solution, corresponding to 0,001 g of boron per litre. Transfer I,0 ml of the stock solution (4.11J) to a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix. Store in a pol
32、ypropylene bottle (5.2). Prepare this solution immediately before use. 1 ml of this standard solution contains 1 pg of boron. 4.12 Curcumin, acetic acid solution, 1,25 g/l. Weigh 0,125 g of curcumin, CH,O(OH)C,H,CH=CHCO,CH, in a polypropylene or quartz vessel, add 60 ml of acetic acid (4.6) and mix.
33、 Heat in a water bath at 40 OC and stir using a magnetic stirrer. After dissolution, cool and transfer to a 100 ml polypropylene volumetric flask. Dilute to the mark with acetic acid and mix. 4.13 Carrier gas, nitrogen, argon or dry air. 5 Apparatus Glassware, polypropylene or quartz equipment rinse
34、d with acetic acid (4.6) then with water and finally dried. All volumetric glassware shall be grade A, in accordance with IS0 3851, IS0 648 or IS0 1042, as appropriate. Ordinary laboratory apparatus and the following shall be used. 5.1 Volumetric flask, of capacity 100 ml. 5.2 Polypropylene bottles,
35、 of capacities 5.3 Distillation apparatus (see annex A), 100 ml and 500 ml. , comprising the following equipment. a) Distillation flask, of capacity 200 ml, made of quartz. b) Reservoir, made of quartz. c) Reflux condenser, made of quartz. d) Receiver, 100 ml quartz beaker marked to indicate a volum
36、e of 35 ml. e) Magnetic stirrer, with rotor covered by polytetrafluoroethene (PTFE). Suitable forms of apparatus are illustrated in annex A. 5.4 Platinum dish or PTFE beaker, of capacity 100 ml. 5.5 Heater, for methanol evaporation. 6 Sampling Carry out sampling in accordance with IS0 14284 or appro
37、priate national standards for steel. 3 ENISO13900:20023OSI )E(7991:00931 0 0SI 7 Procedure 7.1 Test portion Weigh, to the nearest 0,000 1 g, about 050 g of the test sample. 7.2 Blank test and determination of boron in the pure iron (4.1) 7.2.1 Determination of boron in the pure iron (4.1) Prepare tw
38、o distillation flasks 5.3 a). Add 0,250 g of the pure iron (4.1) to one distillation flask and 0,500 g to the other. Treat both as specified in 7.3.1, 7.3.2, 7.3.3 and 7.3.4. Convert the absorbance readings obtained into micrograms of boron by means of the calibration graph (7.4). The mass (m,), exp
39、ressed in micrograms, of boron in 0,500 g of the pure iron (4.1) is given by: m3 =2X(m,-m,) where m6- is the mass, expressed in micrograms, of boron in the 0,500 g test; is the mass, expressed in micrograms, of boron in the 0,250 g test. 7.2.2 Blank test and blank value In parallel with the determin
40、ation of the content and following the same procedure, carry out a blank test using 0,500 g of the pure iron (4.1) and the same quantities of all the reagents. Obtain the absorbance of the blank test and convert it to micrograms of boron by means of the calibration graph (7.4). The blank value(ml) i
41、s obtained by subtracting the mass of boron(mg) in the pure iron used (4.1) from the mass of boron in the blank test(m,). Blank value, m, = m4 - m3 7.3 Determination 7.3.1 Place (4.3). ! 1 Preparation of the test solution the test portion (7.1) in a distillation flask 5.3 a). Add IO ml of hydrochlor
42、ic acid (4.2) and 5 ml of nitric acid Maintain the solution at the ambient temperature (see note I). NOTE 1 Maintaining the temperatures. ambient temperature is most important, in order to avoid possible loss of boron at higher Wait until dissolution is complete, or until the end of effervescence fo
43、r samples which are difficult to dissolve. Then, carefully add IO ml of orthophosphoric acid (4.5) and 5 ml of sulfuric acid (4.4). Heat until white sulfuric acid fumes are generated, swirling from time to time in order to recover any particles attached to the side of the flask. Place the flask on a
44、 heat source permitting a temperature of 290 “C (see note 2) to be obtained in the solution. Maintain heating for 30 min. NOTE 2 The temperature of (290 + 5) “C is obtained by calibrating the heat source with a thermometer, graduated from 0 “C to 350 “C, immersed in a test flask containing the same amounts of dissolution reagents. ENISO13900:20024
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