1、BRITISH STANDARD BS EN ISO 10714:2002 Steel and iron Determination of phosphorus content Phosphovanadomolybdate spectrophotometric method The European Standard EN ISO 10714:2002 has the status of a British Standard ICS 77.040.30 BS EN ISO 10714:2002 This British Standard, having been prepared under
2、the direction 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 40173 1 National foreword This British Standard is the official English language version of EN ISO 107
3、14:2002. It is identical with ISO 10714:1992. 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 committee can be obtained on request to its secreta
4、ry. 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 “Search” facility of the BSI Electronic Catalogu
5、e 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 obligations. aid enquirers to understand th
6、e 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. Summary of pages This document comprises a fron
7、t cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, page ii, pages 1 to 8, the Annex ZA page and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No.
8、Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO10714 July2002 ICS77.040.30 Englishversion SteelandironDeterminationofphophoruscontent Phosphovanadomolybdatespectrophotometricmethod(ISO 10714:1992) AciersetfontesDosageduphosphoreMthodepar spectrophotomtrieauphosphovanadomolybdate(IS
9、O 10714:1992) BestimmungdesPhosphorgehaltesFotometrische BestimmungVanadatomolybdatophosphatVerfahren (ISO10714:1992) ThisEuropeanStandardwasapprovedbyCENon29May2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofa
10、nationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undert
11、heresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spai
12、n,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO10714:2002EINESO0
13、1:4172002(E) 2 Foreword ThetextoftheInternationalStandardfromTechnicalCommitteeISO/TC17“Steel“ofthe InternationalOrganizationforStandardization(ISO)hasbeentakenoverasaEuropean StandardbyTechnicalCommitteeECISS/TC20“Methodsofchemicalanalysisofferrous products“,thesecretariatofwhichisheldbySIS. ThisEu
14、ropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbyJanuary2003,andconflictingnati onal standardsshallbewithdrawnatthelatestbyJanuary2003. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowin
15、gcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,Switzerlandandthe UnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO10714:1992has
16、beenapprovedbyCENasa EuropeanStandardwithoutanymodifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO10714:2002INTERNATIONAL STANDARD 10714 First edi tion 1992-05-15 - - Steel and iron - Determination of phosphorus content - Phosphovanadomolybdate spectrop
17、hotometric method Aciers et fonfes - Uosage du phosphore - Mefhode par spectrophotomktrie au phosphovanadomolybdate - - _._._ -_ _ -.- -_ -.-_ - _ _ - -. ._ - - .- ._. - Reference number ISO 10714:1992(E) ENISO10714:2002OSI )E(2991:41701 droweroF OSI eht( lanoitanretnI noitazinagrO rof )noitazidradn
18、atS si a ediwdlrow noitaredef fo lanoitan sdradnatS seidob OSI( rebmem .)seidob ehT krow fo gniraperp lanoitanretnI sdradnatS si yllamron deirrac tuo hguorht OSI lacinhcet .seettimmoc hcsE rebmem ydob detseretni ni a tcejbus rof hcihw a lacinhcet eettimmoc sah neeb dehsilbatse sah eht thgir ot eb de
19、tneserper no taht .eettimmoc lanoitanretnI ,snoitazinagro -nrevog latnem dna ,latnemnrevog-non ni nosiail htiw ,OSI osla ekat trap ni eht .krow OSI setaroballoc ylesolc htiw eht lanoitanretnI lacinhcetortcelE noissimmoC )CEI( no lla sArettam fo lacinhcetortcele .noitazidradnats tfarD lanoitanretnI s
20、dradnatS detpoda yb eht lacinhcet seettimmoc era detalucric ot eht rebmem seidob rof .gnitov noitacilbuP sa na -retnI lanoitan dradnatS seriuqer lavorppa yb ta tsael 57 % fo eht rebmem seidob gnitsac a .etov lanoitanretnI dradnatS OSI 41701 saw deraperp yb lacinhceT eettimmoC CT/OSI ,71 ,leetS eetti
21、mmoC-buS CS ,1 sdohteM fo noitanimreted fo lacimehC .noitisopmoc ehT noitacilbup fo siht lanoitanretnI dradnatS sevig esir ot eht -lecnac noital fo OSI .4891:2372 sexennA A dna B fo siht lanoitanretnI dradnatS era rof noitamrofni .ylno 0 OSI 2991 llA sthgir .devreser oN trap fo siht noitacilbup yam
22、eb decudorper ro dezilitu ni yna mrof ro yb yna ,snaem einortcele ro ,lacinahcem gnidulcni gniypocotohp dna ,mliforcim tuohtiw noissimrep ni gnitirw morf eht .rehsilbup lanoitanretnI noitazinagrO rof noitazidradnatS esaC elatsoP 65 l 121-HC 1 eveneG 02 l dnalreztiwS detnirP ni dnalreztiwS ii ENISO10
23、714:2002ii-_ - - INTERNATIONAL STANDARD ISO 10714:1992(E) Steel and iron - Determination of phosphorus content - Phosphovanadomolybdate spectrophotometric method 1 Scope This International Standard specifies a spectro- photometric method for the determination of phosphorus in steel and iron with the
24、 following limi- tations. The method is applicable to phosphorus contents between 0,001 0 % (m/m) and 1,0 % (m/rn). Arsenic, hafnium, niobium, tantalum, titanium, and tungsten interfere in determining phosphorus, but the interferences tan be partially overcome by for- mation of complexes and use of
25、small quantities of test portion. Depending on the concentration of the interfering elements, the application ranges and test portions given in table 1 apply. The lower end of the application range tan only be reached in test samples with low contents of the in- terfering elements. 2 Normative refer
26、ences The following Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publi- cation, the editions indicated were valid. All stan- Table 1 dards are subject to revision, and Parties to agreements based on this Inte
27、rnational Standard are encouraged to investigate the possibility of ap- plying the most recent editions of the Standards in- dicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 377-2: 1989, Selection and preparation of samples and test pieces of w
28、rought steels - Part 2: Samples for the determination of the Chemical composition. ISO 385-1:1984, Laborstory glassware - Burettes - Part 1: General requirements. ISO 648:1977, Laboratory glassware - One-mark pipettes. ISO 1042:1983, Laborafory glassware - One-mark volumetric flasks. ISO 3696:1987,
29、Wafer for analyfical laboratory use - Specification and test methods. ISO 5725:1986, Precision of tesf methods - Uefermi- nation of repeatability and reproducibility for a stan- dard test method by inter-laboratory tesfs. Maximum content of the interfering elements, % (r-z?,im) As Hf Nb Ta Ti W 0,05
30、 071 1 071 2 2 02 0,5 5 075 10 8 075 175 10 190 25 25 072 075 5 03 10 8 Test Portion Application range, AW, g % (nt/h?) W 0,001 to 0,010 0,25 0,005 to 0,040 OJO 0,010 to 0,100 0,25 0,100 to l,oo 1 ENISO10714:20021OSI )E(2991:41701 This Solution shall be freshly prepared each day. 3 Principle High an
31、d unstable blank values might be attributable to this reagent in particular. In such a case, Change to another batch. Dissolut mixture. ion of a test portion in an oxidizing acid Fu ming with Per chloric acid and mi um as vola tile chromy I chl oride. removal of chro- 4.9 Ammonium metavanadate, Solu
32、tion. Qissolve 2,5 g of ammonium metavanadate (NHJO,) in water, dilute to 1 000 ml and mix. Complexing of Silicon and the refractory elements with hydrofluoric acid and complexing of the excess of hydrofluoric acid with orthoboric acid. 4.10 Sodium nitrite, solution. Conversion of phosphorus to phos
33、phovan molybdate in per ,chloric and nitric acid Solution. ado- Dissolve 50 g of sodium nitrite (NaNO,) in water, di- lute to 1 000 ml and mix. Extraction of phosphovanadomolybdate by 4-methyl-2-pentanone with citric acid present to complex arsenic. 4.11 Tetrafluoroboric acid, solution. Dissolve 75
34、g of or-thoboric acid (H,BO,) in 600 ml of water in a plastic beaker. Add 50 ml of hydrofluoric acid (4.5) dilute to 1 000 and mix. The solution tan be gently boric acid tends to precipitate. Keep the Solution in a plastic bettle. ml with water heated if the Spectrophotometric measurement at a wavel
35、ength of 355 nm. 4.12 Phosphorus, Standard solutions . 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 2 water as specified in ISO 3696. 4.12.1 Stock solution, corresponding to 1 g of P per Iitre. Verify by blank tests (7.2) th
36、at the relevant reagents are free from phosphorus or of very low phosphorus content. Whenever necessary, the results shall be corrected accordingly. Grades givinq high blank values (above 10 pg) are unsuitable -and shall be discarded. Weigh, to the nearest 0,000 1 g, 4,393 6 g of potass- ium dihydro
37、gen orthophosphate (KH,PO,) previously dried to constant mass at 110 C and cooled in a desiccator. 4.1 Hydrochlorit acid, 3 about 1,19 g/ml. Transfer to a 1 000 ml one-mal-k volumetric flask, dissolve in water. dilute to the mark and mix. 4.2 Nitrit acid, 3 about 1,40 g/ml. 1 ml of this stock Soluti
38、on contains 1 mg of P. 4.3 Nitrit acid, 3 about 1,40 g/ml, diluted 1 + 4. 4.12.2 Standard Solution, corresponding to 10 mg of P per litre. 4.4 Perchlorit acid, p about 1,54 g/ml. Transfer IO,0 ml of the stock Solution (4.12.1) to a 1 000 ml one-mark volumetric flask, dilute to the mark with water an
39、d mix. 4.5 Hydrofluoric acid, 40 % (n/nz), c) about 1,14 g/ml. Prepare this Standard Solution just before use. 4.6 Citric acid, Solution. 1 mf of this Standard Solution contains 10 ug of P. Dissolve 500 g of citric acid monohydrate (H,C,O,.H,O) in water, dilute to 1 000 ml and mix. 5 Apparatus 4.7 4
40、-Methyl-2-pentanone (isobutyl methyl ketone). All volumetric glassware shall be class A, in ac- cordante with ISO 385-1, ISO 648 or ISO 1042 as The Same batch of 4-methyl-2-pentanone shall be used for an alysin g a series of samples. appropriate. Ordinary laboratory apparatus, and 4.8 Hexa-ammonium
41、heptamolybdate, solution. 5.1 Spectrophotometer, equipped to absorbance at a wavelength of 355 nm. measure Dissolve 150 g of hexa-ammonium heptamolybdate tetrahydrate (NH,),Mo,0,.4H,OI in water, dilute to 1 000 ml and mix. Using the slitwidth recommended by the manufac- ENISO10714:20022OSI )E(2991:4
42、1701 turer and 4-methyl-2-pentanone (4.7) as the com- pensating solution, measure the absorbance of the colour-developed and extracted blank Solution (see 7.3.2) at a wavelength of about 340 nm. Then gradu- ally increase the wavelength until maximum absorbance is obtained (this is generally at a wav
43、e- length of 355 nm, see note 1). Use this wavelength for the determination. 6 Sampling Carry out sampling in accordance with ISO 377-2 or appropriate national Standards for steel and iron. 7 Procedure 7.1 Test Portion NOTE 1 355 nm is not the wavelength of the maximum absorption spectrum from the c
44、omplex. It is not possible to use the maximum Point since the 4-methyl-2-pentanone Starts to absorb the light at a lower wavelength, where a maximum absorbance value is obtained. 355 nm is selec- ted to give the highest absorption without giving negative absorption values for low concentration due t
45、o the light absorption of the solvent. Weigh, to the nearest O,l mg, a test Portion of the Sample according to table2. 7.2 Blank test 5.2 Polytetrafluoroethylene (PTFE) beakers, or perfluoroalkoxy (PFA) beakers (see note 2), with graphite bases. In parallel with the determination and following the S
46、ame procedure, carry out a blank test using the Same quantities of all the reagents. 7.3 Determination Clean the beakers thoroughly before the analysis by filling with hydrochloric acid, p about IJ9 g/ml, di- luted 1 + 1, and boiling for about 2 min. Then rinse well with water. NOTE 2 PFA beakers ar
47、e recommended in this Inter- national Standard. They are specially constructed for fuming of acids up to 280 OC. 5.3 Heating Source, with controllable surface tem- perature. 7.3.1 Preparation of the test Solution 7.3.1.1 For phosphorus contents up to 0,l % (m/m) Place the test Portion (7.1) in a bea
48、ker (5.2). Add 5 ml of nitric acid (4.2) and 5 ml of hydrochloric acid (4.1). For samples containing high amounts of niobium and/or tantalum, also add 7 ml of hydrofluoric acid (4.5). Cover the beaker with a PTFE watch-glass and heat gently on a heating Source (5.3) until the reaction ceases. Table 2 , Expected phosphorus content Maximum content of the interfering elements, O/o (m/nz) Test Portion -
