《BS-EN-ISO-10714-2002.pdf》由会员分享,可在线阅读,更多相关《BS-EN-ISO-10714-2002.pdf(16页珍藏版)》请在三一文库上搜索。
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 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+0
2、0:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 10714:2002 This British Standard, having been prepared under 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
3、 0 580 40173 1 National foreword This British Standard is the official English language version of EN ISO 10714:2002. 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 respo
4、nsibility to: A list of organizations represented on this committee 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 “In
5、ternational Standards Correspondence Index”, or by using the “Search” 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
6、 a British Standard does not of itself confer immunity from legal 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 internati
7、onal and European developments and promulgate them in the UK. Summary 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 8, the Annex ZA page and a back cover. The BSI copyright date displaye
8、d in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10714 July 200
9、2 ICS 77.040.30 English version Steel and iron - Determination of phophorus content - Phosphovanadomolybdate spectrophotometric method (ISO 10714:1992) Aciers et fontes - Dosage du phosphore - Mthode par spectrophotomtrie au phosphovanadomolybdate (ISO 10714:1992) Bestimmung des Phosphorgehaltes - F
10、otometrische Bestimmung - Vanadatomolybdatophosphat-Verfahren (ISO 10714:1992) This European Standard was approved by CEN on 29 May 2002. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a nationa
11、l standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any oth
12、er language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Gre
13、ece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2002 CENAll right
14、s of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 10714:2002 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI I NESO 01:4172002 (E) 2 Foreword The text of the International Standard
15、from Technical Committee ISO/TC 17 “Steel“ of the International Organization for Standardization (ISO) has been taken over as a European Standard by Technical Committee ECISS/TC 20 “Methods of chemical analysis of ferrous products“, the secretariat of which is held by SIS. This European Standard sha
16、ll be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2003, and conflicting national standards shall be withdrawn at the latest by January 2003. According to the CEN/CENELEC Internal Regulations, the national standards o
17、rganizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsemen
18、t notice The text of the International Standard ISO 10714:1992 has been approved by CEN as a European Standard without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN ISO 10714:2002 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19
19、16:02:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD 10714 First edi tion 1992-05-15 - - Steel and iron - Determination of phosphorus content - Phosphovanadomolybdate spectrophotometric method Aciers et fonfes - Uosage du phosphore - Mefhode par spectrophotomktrie au phosphovan
20、adomolybdate - - _._._ -_ _ -.- -_ -.-_ - _ _ - -. ._ - - .- ._. - Reference number ISO 10714:1992(E) EN ISO 10714:2002 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI OSI )E(2991:41701 droweroF OSI eht( lanoitanretnI noitazinagrO rof )noita
21、zidradnatS 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 o
22、t eb detneserper 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 lanoitan
23、retnI sdradnatS 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 ,leet
24、S eettimmoC-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 noitacilb
25、up yam 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
26、EN ISO 10714:2002 ii Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI -_ - - INTERNATIONAL STANDARD ISO 10714:1992(E) Steel and iron - Determination of phosphorus content - Phosphovanadomolybdate spectrophotometric method 1 Scope This Interna
27、tional Standard specifies a spectro- photometric method for the determination of phosphorus in steel and iron with the 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 interf
28、ere in determining phosphorus, but the interferences tan be partially overcome by for- mation of complexes and use of 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 ap
29、plication range tan only be reached in test samples with low contents of the in- terfering elements. 2 Normative references The following Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publi- cation, the editio
30、ns indicated were valid. All stan- Table 1 dards are subject to revision, and Parties to agreements based on this International 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
31、of currently valid International Standards. ISO 377-2: 1989, Selection and preparation of samples and test pieces of wrought 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, Labor
32、atory glassware - One-mark pipettes. ISO 1042:1983, Laborafory glassware - One-mark volumetric flasks. ISO 3696:1987, 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
33、 test method by inter-laboratory tesfs. Maximum content of the interfering elements, % (r-z?,im) As Hf Nb Ta Ti W 0,05 071 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
34、,100 to l,oo 1 EN ISO 10714:2002 1 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI OSI )E(2991:41701 This Solution shall be freshly prepared each day. 3 Principle High and unstable blank values might be attributable to this reagent in partic
35、ular. 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, Solution. Qissolve 2,5 g of ammonium metavanadate (NHJO,) in water, dilute
36、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 phosphovan molybdate in per ,chloric and nitric acid Solution. ado- Dissolv
37、e 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 g of or-thoboric acid (H,BO,) in 600 ml of water in a plastic beaker. A
38、dd 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 wavelength of 355 nm. 4.12 Phosphorus, Standard solutions . 4 Reagents Durin
39、g 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) that the relevant reagents are free from phosphorus or of very low phosph
40、orus 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 dihydrogen orthophosphate (KH,PO,) previously dried to constant mass at 110 C
41、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 Solution contains 1 mg of P. 4.3 Nitrit acid, 3 about 1,40 g/ml, diluted 1 +
42、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 and mix. 4.5 Hydrofluoric acid, 40 % (n/nz), c) about 1,14 g/ml. Prepare
43、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-Methyl-2-pentanone (isobutyl methyl ketone). All volumetric glassware
44、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 heptamolybdate, solution. 5.1 Spectrophotometer, equipped to absorbance
45、 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- EN ISO 10714:2002 2 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 16:02:35 GMT+00:00 2006,
46、Uncontrolled Copy, (c) BSI OSI )E(2991:41701 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
47、 is obtained (this is generally at a wave- 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 th
48、e maximum absorption spectrum from the complex. 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 absor
49、ption values for low concentration due to 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 Same procedure, carry out a blank test using the Same quantities of all the reagents. 7.3 Determination Clean the beakers thoroughly before the analy
链接地址:https://www.31doc.com/p-3747022.html