SIST EN ISO 10714:2003

SLOVENSKI STANDARD
01-april-2003
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VSHNWURIRWRPHWULMVNDPHWRGD,62
Steel and iron - Determination of phophorus content - Phosphovanadomolybdate
spectrophotometric method (ISO 10714:1992)
Bestimmung des Phosphorgehaltes - Fotometrische Bestimmung -
Vanadatomolybdatophosphat-Verfahren (ISO 10714:1992)
Aciers et fontes - Dosage du phosphore - Méthode par spectrophotométrie au
phosphovanadomolybdate (ISO 10714:1992)
Ta slovenski standard je istoveten z: EN ISO 10714:2002
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 10714
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2002
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 - Méthode par Bestimmung des Phosphorgehaltes - Fotometrische
spectrophotométrie au phosphovanadomolybdate (ISO Bestimmung - Vanadatomolybdatophosphat-Verfahren
10714:1992) (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 national 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 other 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, Greece,
Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
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Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 10714:2002 E
worldwide for CEN national Members.

Foreword
The text of the International Standard 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 shall 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 organizations 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.
Endorsement 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).
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions
of any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated by
(mod.), the relevant EN/HD applies.
Publication Year Title EN/HD Year
ISO 1042 1998 Laboratory glassware - One-mark volumetric EN ISO 1042 1999
flasks
ISO 3696 1987 Water for analytical laboratory use - EN ISO 3696 1995
Specification and test methods
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 phosphovanadomolybdate
-.- - _._._~
-_ _ -.-
Reference number
---_ -.-___
-. _ _ - -. ._ - - .- ._. --
ISO 10714:1992(E)
ISO 10714:1992(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established has the right to be
represented on that committee. International organizations, govern-
mental and non-governmental, in liaison with ISO, also take part in the
work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matterAs of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an Inter-
national Standard requires approval by at least 75 % of the member
bodies casting a vote.
International Standard ISO 10714 was prepared by Technical Committee
ISO/TC 17, Steel, Sub-Committee SC 1, Methods of determination of
Chemical composition.
The publication of this International Standard gives rise to the cancel-
lation of ISO 2732:1984.
Annexes A and B of this International Standard are for information only.
0 ISO 1992
All rights reserved. No part of this publication may be reproduced or utilized in any form
or by any means, electronie or mechanical, including photocopying and microfilm, without
permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-121 1 Geneve 20 l Switzerland
Printed in Switzerland
ii
_-- --- -
ISO 10714:1992(E)
INTERNATIONAL STANDARD
- Determination of phosphorus content -
Steel and iron
Phosphovanadomolybdate spectrophotometric method
dards are subject to revision, and Parties to
1 Scope
agreements based on this International Standard
are encouraged to investigate the possibility of ap-
This International Standard specifies a spectro-
plying the most recent editions of the Standards in-
photometric method for the determination of
dicated below. Members of IEC and ISO maintain
phosphorus in steel and iron with the following limi-
registers of currently valid International Standards.
tations.
The method is applicable to phosphorus contents ISO 377-2: 1989, Selection and preparation of samples
and test pieces of wrought steels - Part 2: Samples
between 0,001 0 % (m/m) and 1,0 % (m/rn).
for the determination of the Chemical composition.
Arsenic, hafnium, niobium, tantalum, titanium, and
tungsten interfere in determining phosphorus, but
ISO 385-1:1984, Laborstory glassware - Burettes -
the interferences tan be partially overcome by for-
Part 1: General requirements.
mation of complexes and use of small quantities of
test portion. Depending on the concentration of the
ISO 648:1977, Laboratory glassware - One-mark
interfering elements, the application ranges and test
pipettes.
portions given in table 1 apply.
ISO 1042:1983, Laborafory glassware - One-mark
The lower end of the application range tan only be
volumetric flasks.
reached in test samples with low contents of the in-
terfering elements.
ISO 3696:1987, Wafer for analyfical laboratory use -
Specification and test methods.
2 Normative references
ISO 5725:1986, Precision of tesf methods - Uefermi-
The following Standards contain provisions which, nation of repeatability and reproducibility for a stan-
through reference in this text, constitute provisions dard test method by inter-laboratory tesfs.
of this International Standard. At the time of publi-
cation, the editions indicated were valid. All stan-
Table 1
Maximum content of the interfering elements, % (r-z?,im)
Test Portion Application range, AW,
As Hf Nb Ta Ti W % (nt/h?)
g
0,001 to 0,010
0,05 071 1 071 2 2 W
0,005 to 0,040
02 0,5 5 075 10 8 0,25
25 25 OJO 0,010 to 0,100
075 175 10 190
5 03 10 8 0,25 0,100 to l,oo
072 075
ISO 10714:1992(E)
This Solution shall be freshly prepared each day.
3 Principle
High and unstable blank values might be attributable
ion of a test portion in an oxidizing acid
Dissolut
to this reagent in particular. In such a case, Change
mixture.
to another batch.
removal of chro-
Fu ming with chloric acid and
Per
4.9 Ammonium metavanadate, Solution.
oride.
mi um as vola tile chromy I chl
Qissolve ammonium metavanadate
2,5 g of
Complexing of Silicon and the refractory elements
(NHJO,) in water, dilute to 1 000 ml and mix.
with hydrofluoric acid and complexing of the excess
of hydrofluoric acid with orthoboric acid.
4.10 Sodium nitrite, solution.
phosphorus to phosphovan ado-
Conversion of
,chloric and nitric acid Solution.
molybdate in per 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
4.11 Tetrafluoroboric acid, solution.
complex arsenic.
Dissolve 75 g of or-thoboric acid (H,BO,) in 600 ml
Spectrophotometric measurement at a wavelength
of water in a plastic beaker. Add 50 ml of
of 355 nm.
hydrofluoric acid (4.5) dilute to 1 000 ml with water
and mix. The solution tan be gently heated if the
boric acid tends to precipitate.
4 Reagents
Keep the Solution in a plastic bettle.
During the analysis, unless otherwise stated, use
only reagents of recognized analytical grade and
4.12 Phosphorus, Standard solutions .
only grade 2 water as specified in ISO 3696.
Verify by blank tests (7.2) that the relevant reagents 4.12.1 Stock solution, corresponding to 1 g of P per
are free from phosphorus or of very low phosphorus Iitre.
content. Whenever necessary, the results shall be
Weigh, to the nearest 0,000 1 g, 4,393 6 g of potass-
corrected accordingly. Grades givinq high blank
ium dihydrogen orthophosphate (KH,PO,) previously
values (above 10 pg) are unsuitable -and shall be
dried to constant mass at 110 ‘C and cooled in a
discarded.
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 + 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
4.5 Hydrofluoric acid, 40 % (~n/nz), c) about
mark with water and mix.
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.
acid monohydrate
Dissolve 500 g of citric
(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 shall be class A, in ac-
cordante with ISO 385-1, ISO 648 or ISO 1042 as
Same of 4-methyl-2-pentanone shall be
The batch
appropriate.
used for an alysin g a series of samples.
Ordinary laboratory apparatus, and
4.8 Hexa-ammonium heptamolybdate, solution.
5.1 Spectrophotometer, equipped to measure
Dissolve 150 g of hexa-ammonium heptamolybdate
absorbance at a wavelength of 355 nm.
tetrahydrate [(NH,),Mo,0,,.4H,OI in water, dilute to
Using the slitwidth recommended by the manufac-
1 000 ml and mix.
ISO 10714:1992(E)
turer and 4-methyl-2-pentanone (4.7) as the com-
6 Sampling
pensating solution, measure the absorbance of the
colour-developed and extracted blank Solution (see
Carry out sampling in accordance with ISO 377-2 or
7.3.2) at a wavelength of about 340 nm. Then gradu-
appropriate national Standards for steel and iron.
ally increase the wavelength until maximum
absorbance is obtained (this is generally at a wave-
7 Procedure
length of 355 nm, see note 1). Use this wavelength
for the determination.
7.1 Test Portion
NOTE 1 355 nm is not the wavelength of the maximum
absorption spectrum from the complex. It is not possible
Weigh, to the nearest O,l mg, a test Portion of the
to use the maximum Point since the 4-methyl-2-pentanone
Sample according to table2.
Starts to absorb the light at a lower wavelength, where a
maximum absorbance value is obtained. 355 nm is selec-
7.2 Blank test
ted to give the highest absorption without giving negative
absorption values for low concentration due to the light
absorption of the solvent. In parallel with the determination and following the
Same procedure, carry out a blank test using the
Same quantities of all the reagents.
5.2 Polytetrafluoroethylene (PTFE) beakers, or
perfluoroalkoxy (PFA) beakers (see note 2), with
7.3 Determination
graphite bases.
Clean the beakers thoroughly before the analysis by 7.3.1 Preparation of the test Solution
filling with hydrochloric acid, p about IJ9 g/ml, di-
luted 1 + 1, and boiling for about 2 min. Then rinse
7.3.1.1 For phosphorus contents up to 0,l % (m/m)
well with water.
Place the test Portion (7.1) in a beaker (5.2). Add
NOTE 2 PFA beakers are recommended in this Int
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