BS ISO 4942:201 6

BSI Standards Publication

Steels and irons —

Determination of vanadium
content — N-BPHA
spectrophotometric method
BS ISO 4942:201 6 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of ISO 4942:201 6.
It supersedes BS 6200-3.34.2:1 989 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee ISE/1 02, Methods of Chemical Analysis for Iron and Steel.
A list of organizations represented on this committee can be
obtained on request to its secretary.
This publication does not purport to include all the necessary
provisions of a contract. Users are responsible for its correct
application.
© The British Standards Institution 201 6.
Published by BSI Standards Limited 201 6
ISBN 978 0 580 81 537 9
ICS 77.080.01
Compliance with a British Standard cannot confer immunity from
legal obligations.
This British Standard was published under the authority of the
Standards Policy and Strategy Committee on 31 July 201 6.
Amendments/corrigenda issued since publication
Date Text affected
INTERNATIONAL
BS ISO 4942:201 6
ISO
STANDARD 4942

Second edition
2016-07-01

Steels and irons — Determination

of vanadium content — N-BPHA
spectrophotometric method
Aciers et fontes — Détermination de la teneur en vanadium —
Méthode spectrophotométrique au N-BPHA

Reference number
ISO 4942:2016(E)

© ISO 2016
BS ISO 4942:201 6
ISO 4942:2016(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part o f this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country o f
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www.iso.org

ii © ISO 2016 – All rights reserved

 BS ISO 4942:201 6
ISO 4942:2016(E)

Contents Page
Foreword ........................................................................................................................................................................................................................................ iv
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Terms and definitions ..................................................................................................................................................................................... 1
4 Principle ........................................................................................................................................................................................................................ 1
5 Reagents ........................................................................................................................................................................................................................ 1
6 Apparatus ..................................................................................................................................................................................................................... 3
7 Sampling........................................................................................................................................................................................................................ 3
8 Procedure ..................................................................................................................................................................................................................... 3
8.1 Test portion ................................................................................................................................................................................................ 3
8.2 Blank test ..................................................................................................................................................................................................... 3
8.3 Determination ......................................................................................................................................................................................... 4
8.3.1 Preparation of the test solution .......................................................................................................................... 4
8.3.2 Oxidation of vanadium................................................................................................................................................ 4
8.3.3 Colour development and extraction................................................................................................................ 4
8.3.4 Spectrophotometric measurements ............................................................................................................... 4
8.4 Establishment of the calibration curve .............................................................................................................................. 5
8.4.1 Preparation of the calibration solutions ...................................................................................................... 5
8.4.2 Spectrophotometric measurements ............................................................................................................... 5
8.4.3 Plotting of the calibration curve ......................................................................................................................... 5
9 Expression of results ........................................................................................................................................................................................ 5
9.1 Method of calculation ........................................................................................................................................................................ 5
9.2 Precision ....................................................................................................................................................................................................... 6
10 Special cases .............................................................................................................................................................................................................. 7
11 Test report................................................................................................................................................................................................................... 7
Annex A (informative) Additional information on the international interlaboratory test.......................... 8
Annex B (informative) Graphical representation of precision data .................................................................................... 9
Bibliography ............................................................................................................................................................................................................................. 10

© ISO 2016 – All rights reserved iii

BS ISO 4942:201 6
ISO 4942:2016(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work o f preparing International Standards is normally carried out
through ISO technical committees. Each 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, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o f
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
di fferent types o f ISO documents should be noted. This document was dra fted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some o f the elements o f this document may be the subject o f
patent rights. ISO shall not be held responsible for identi fying any or all such patent rights. Details o f
any patent rights identified during the development o f the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is in formation given for the convenience o f users and does not
constitute an endorsement.
For an explanation on the meaning o f ISO specific terms and expressions related to con formity assessment,
as well as information about ISO’s adherence to the World Trade Organization (WTO) principles in the
Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.
The committee responsible for this document is ISO/TC 17, Steel, Subcommittee SC 1, Methods of
determination of chemical composition .

This second edition cancels and replaces the first edition (ISO 4942:1988), which has been technically
revised.

iv © ISO 2016 – All rights reserved

 BS ISO 4942:201 6
INTERNATIONAL STANDARD ISO 4942:2016(E)

Steels and irons — Determination of vanadium content —

N-BPHA spectrophotometric method

1 Scope
This document specifies an N-benzoylphenylhydroxylamine (N-BPHA) spectrophotometric method for
the determination of vanadium in steels and cast irons.
This document is applicable to vanadium contents between 0,005 % and 0,50 % (mass fraction).
2 Normative references
The following documents are re ferred to in text in such a way that some or all o f their content
constitutes requirements o f this document. For dated re ferences, only the edition cited applies. For
undated re ferences, the latest edition o f the re ferenced document (including any amendments) applies.
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition

3 Terms and definitions

No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
Dissolution of a test portion with appropriate acids.
Addition of orthophosphoric acid to an aliquot of the sample solution to prevent the interference of iron,
and addition of potassium permanganate to oxidize vanadium to the pentavalent state.
Selective reduction o f excess permanganate by sodium nitrite, in the presence o f urea and treatment
with N-BPHA and hydrochloric acid to form a complex, followed by extraction o f the complex with
trichloromethane.
Spectrophotometric measurement o f the absorbance at approximately 535 nm.

5 Reagents
During analysis, unless otherwise stated, use only reagents o f recognized analytical grade and only
grade 2 water as specified in ISO 3696 or water o f equivalent purity.

© ISO 2016 – All rights reserved 1

BS ISO 4942:201 6
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5.1 Hydrochloric acid, ρ approximately 1,19 g/ml.

5.2 Hydrochloric acid, ρ approximately 1,19 g/ml, diluted 4 + 1.

Add 400 ml o f hydrochloric acid (5.1) to 100 ml of water.

5.3 Nitric acid, ρ approximately 1,40 g/ml.

5.4 Perchloric acid, ρ approximately 1,67 g/ml.

WARNING — Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous
fumes or organic material in general.

5.5 ,
Orthophosphoric acid ρ approximately 1,71 g/ml.

5.6 ,
Orthophosphoric acid ρ approximately 1,71 g/ml, diluted 1 + 1.
Add 250 ml of orthophosphoric acid (5.5) to 250 ml of water.
5.7 Hydrochloric/nitric acids mixture , 3 + 1.
Mix 300 ml o f hydrochloric acid (5.1) with 100 ml of nitric acid (5.3).
Prepare this mixture immediately prior to use.
5.8 Hydrogen peroxide , 300 g/l solution.
5.9 Sodium nitrite , 3 g/l solution.
5.10 Urea , 250 g/l solution.
5.11 Sodium tripolyphosphate (Na 5 P 3 O 10 ) , 100 g/l solution.
5.12 Potassium permanganate , 3 g/l solution.
5.13 Trichloromethane (chloroform) .
5.14 N-benzoylphenylhydroxylamine [C 6 H 5 CON(OH)C 6 H 5 ] , 2,5 g/l solution in trichloromethane.
Dissolve 0,25 g of N-BPHA in 100 ml of trichloromethane (5.13).
This solution shall be stored in a brown bottle. Otherwise, it shall be freshly prepared.

5.15 Iron , 10 g/l solution.

Weigh, to the nearest 1 mg, 5,0 g of pure iron (free from vanadium or with a vanadium content as low as
possible and exactly known). Trans fer into a 500 ml beaker, cover with a watch-glass and add 100 ml o f
the hydrochloric/nitric acids mixture (5.7).
A fter e ffervescence has ceased, heat gently to complete the dissolution.
Add 100 ml of perchloric acid (5.4) and raise the temperature until white perchloric acid fumes appear
and then reflux in the beaker. Continue fuming for about 3 min.
Cool, add 100 ml o f hot water and shake to dissolve salts. Add a few drops o f hydrogen peroxide (5.8),
heat gradually to boiling and maintain at the boil for about 2 min.

2 © ISO 2016 – All rights reserved

 BS ISO 4942:201 6
ISO 4942:2016(E)

Cool and trans fer into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix.

5.16 Vanadium standard solution , 1,0 g/l.

Dry several grams o f ammonium metavanadate (NH 4VO 3 ) in an oven at 100 °C to 105 °C for at least 1 h
and cool to room temperature in a desiccator.
A drying temperature over 110 °C will cause the decomposition o f ammonium metavanadate. Maintain
the drying temperature exactly as specified.
Weigh, to the nearest 1 mg, 2,296 g of the dried product, transfer into a 600 ml beaker, add 400 ml of
hot water and heat gently until the product is completely dissolved.
Cool, trans fer into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix.
1 ml of this standard solution contains 1,0 mg of vanadium.
5.17 Vanadium standard solution , 50 mg/l.
Transfer 5,0 ml of the vanadium standard solution (5.16) into a 100 ml one-mark volumetric flask,
dilute to the mark with water and mix.
1 ml of this standard solution contains 50 µg of vanadium.
6 Apparatus
All volumetric glassware shall be grade A, in accordance with ISO 648 or ISO 1042, as appropriate.
Ordinary laboratory equipment and the following.

6.1 Spectrophotometer , equipped to measure absorbance at a wavelength of 535 nm, with cells of
1 cm optical path length.
7 Sampling
Carry out sampling in accordance with ISO 14284 or appropriate national standards for steels and irons.

8 Procedure

8.1 Test portion

Weigh, to the nearest 1 mg, a test portion of the sample according to Table 1.
Table 1 — Test portion

Expected vanadium content Test portion

% (mass fraction) (g)
0,005 to 0,10 1,0
0,10 to 0,20 0,50
0,20 to 0,50 0,20
8.2 Blank test
Carry out a blank test simultaneously with the determination, following the same procedure and using
the same quantities of all reagents as used for the determination (see 8.3.2 and 8.3.3) but replacing the
test solution by the iron solution (5.15).

© ISO 2016 – All rights reserved 3

BS ISO 4942:201 6
ISO 4942:2016(E)

8.3 Determination

8.3.1 Preparation of the test solution

Transfer the test portion (8.1) (see 10.1) to a 250 ml beaker, cover with a watch-glass and add 20 ml
to 30 ml o f the hydrochloric/nitric acids mixture (5.7 ). When e ffervescence has ceased, heat gently to
complete the dissolution.
Add 15 ml to 20 ml of perchloric acid (5.4), raise the temperature so that white perchloric acid fumes
appear and reflux in the beaker and continue fuming for about 3 min.
NOTE In the case o f cast irons, fuming with perchloric acid for about 3 min is not always su fficient to
decompose carbides. Total decomposition is only complete when heating is continued until no more fumes are
visible in the beaker and crystallization has occurred. A fter cooling, add about 30 ml o f water and 10 ml o f
perchloric acid (5.4) be fore continuing as described below from “Add hydrogen peroxide (5.8)...”.
Cool, add about 30 ml o f hot water and shake to dissolve salts. Add hydrogen peroxide (5.8) dropwise to
reduce chromium, gradually heat to boiling and continue for 1 min to 2 min to decompose the excess o f
hydrogen peroxide.
A fter cooling, filter through a medium texture filter paper and collect the filtrate in a 100 ml one-
mark volumetric flask. Wash the filter paper several times with hot water. Dilute to the mark with
water and mix.
8.3.2 Oxidation of vanadium

Transfer 25,0 ml of the test solution (8.3.1) into a 125 ml separating funnel. Add 2,0 ml of orthophosphoric
acid (5.6) (see 10.2 and 10.3) and 5,0 ml of water and swirl.
Add 0,8 ml of potassium permanganate solution (5.12), swirl and allow to stand for 4 min. Add 5,0 ml
of urea solution (5.10) and then add 1,0 ml of sodium nitrite solution (5.9), drop by drop while swirling.
Even if, after the addition of 1,0 ml of sodium nitrite solution (5.9), the solution still appears slightly
pink, proceed, without any further addition o f sodium nitrite solution, to 8.3.3.
Allow to stand for 1 min.
8.3.3 Colour development and extraction

Add 25,0 ml o f hydrochloric acid (5.2) and 10,0 ml of N-BPHA (5.14) and shake for 45 s.
When the layers have separated, draw o ff the organic phase, filtering through a dry filter paper fitted
in an ordinary funnel, or through absorbent cotton fitted in the stem o f a separating funnel, into a dry
50 ml one-mark volumetric flask.
Retain the aqueous phase.
Add 10,0 ml of trichloromethane (5.13) to the aqueous phase remaining in the separating funnel and
shake for 30 s. Allow to settle, combine the organic phase with the main extract, dilute to the mark with
trichloromethane (5.13) and mix (see the following paragraph).
To ensure the same colour development conditions for the test and the calibration solutions, take each
solution one by one through the steps from the vanadium oxidation (8.3.2) to the extraction (8.3.3).
Avoid batch colour development and carry out each step without delay, unless otherwise specified.

8.3.4 Spectrophotometric measurements

Measure the absorbance of the test solutions at a wavelength of about 535 nm in cells of 1 cm path length,
after having adjusted the spectrophotometer (6.1) to the zero absorbance against trichloromethane (5.13).

4 © ISO 2016 – All rights reserved

 BS ISO 4942:201 6
ISO 4942:2016(E)

8.4 Establishment of the calibration curve

8.4.1 Preparation of the calibration solutions

Transfer 25,0 ml portions of iron solution (5.15) into a series of 125 ml separating funnels. Add the
volumes of vanadium standard solution (5.17) and of water shown in Table 2, swirl and proceed as
8.3.2 and 8.3.3
s p e ci fie d i n f f
, but om it the add ition o 8.3.2.
5 ml o water s p e c i fie d i n

Table 2 — Composition of the calibration solutions

Vanadium standard solution (5.17) Water Corresponding vanadium concentration

ml ml µg/ml
0 5,0 0
0,5 4,5 0,5
1,0 4,0 1,0
2,0 3,0 2,0
4,0 1,0 4,0
5,0 0 5,0
8.4.2 Spectrophotometric measurements

Measure the absorbance of each solution at a wavelength of about 535 nm, in cells of 1 cm path length,
f 6.1) to the zero absorbance against the zero member of
a ter havi ng adj u s te d the s p e c tropho tome ter (

the calibration solutions.

8.4.3 Plotting of the calibration curve

E s tabl i sh the c a l ibration c u r ve b y plo tti ng the ab s orb a nce va lue s agai n s t the vanad iu m concentration s ,

expressed in micrograms per millilitre, in the calibration solutions.

9 Expression of results

9.1 Method of calculation

Convert the absorbance measured in 8.3.4 to the corresponding concentration, expressed in micrograms
f
p er m i l l i l itre o 8.4.3).
va nad ium i n the colour- develop e d te s t s olution, b y u s i ng the ca l ibration c u r ve (

The vanadium content, mV, f

expre s s e d as a ma s s Formulae (1) to (3):
rac tion p ercentage (%) , i s given b y

mV = ( C V1 − C V0 ) ×
V0 × Vt × 100 + C Fe
1
× (1)
10 V1 m m
6

m V = ( C V1 − C V0 ) × 1 6 × 100 × 50 × 100 + C Fe (2)

10 25 m m
m V = ( C V1 − C V0 ) × 1 + C Fe (3)
50 m m

© ISO 2016 – All rights reserved 5

BS ISO 4942:201 6
ISO 4942:2016(E)

where
V0 is the volume of the test solution (8.3.1), in ml;
V1 is the volume of the aliquot portion (8.3.2), in ml;
Vt is the volume of the colour-developed test solution (8.3.3), in ml;
CV0 is the concentration o f vanadium in the blank test solution, in μg/ml;
CV1 is the concentration o f vanadium in the test solution, in μg/ml;
m is the mass of the test portion (8.1), in g;
CFe is the vanadium content in the iron used in the blank test, expressed as mass fraction in %.
9.2 Precision
A planned trial o f this method was carried out by 11 laboratories, at seven levels o f vanadium, each
laboratory making three determinations at each level (see Notes 1 and 2).
The test samples used are listed in Annex A.
The results obtained were treated statistically in accordance with ISO 5725:19861) (see Note 3).
The data obtained showed logarithmic relationships between vanadium content and the repeatability,
r, and reproducibilities, Rw and R , of the test results, as summarized in Table 3.

Table 3 — Repeatability limit and reproducibility limits

Vanadium content Repeatability limit Reproducibility limits

% (mass fraction) r Rw R
0,005 0,001 0 0,001 1 0,002 1
0,010 0,001 6 0,001 8 0,003 2
0,020 0,002 4 0,002 8 0,004 9
0,050 0,004 2 0,005 4 0,008 7
0,100 0,006 6 0,008 7 0,013 4
0,200 0,010 2 0,014 1 0,020 7
0,500 0,018 1 0,026 7 0,036 7
A graphical representation of the data is given in Figure B.1.
NOTE 1 Two o f the three determinations were carried out under repeatability conditions as defined in
ISO 5725:19861) , i.e. one operator, same apparatus, identical operating conditions (same calibration) and a
minimum period of time.
NOTE 2 The third determination was carried out at a di fferent time (di fferent day) by the same operator as in
Note 1 above, using the same apparatus but with a new calibration.
NOTE 3 From the values obtained on day 1, the repeatability, r, and reproducibility, R , were calculated using
the procedure specified in ISO 5725:19861) . From the first value obtained on day 1 and the value obtained on
day 2, the within-laboratory reproducibility, Rw, was calculated.

1) Withdrawn. (Replaced with the ISO 5725 series.)

6 © ISO 2016 – All rights reserved
 BS ISO 4942:201 6
ISO 4942:2016(E)

10 Special cases

10.1 For test portions containing tungsten, transfer the test portion (8.1) into a 250 ml beaker, cover
with a watch-glass and add 15 ml to 20 ml of perchloric acid (5.4), 5 ml of orthophosphoric acid (5.5) and
3 ml to 5 ml of nitric acid (5.3 ) . H eat gently to co mp lete the dis s o lutio n, increas e the temp erature until

white p erchlo ric acid fumes reflux in the b eaker and co ntinue fo r ab o ut 3 min.

10.2 For test portions containing tungsten, omit the addition of 2,0 ml of orthophosphoric acid (5.6).
10.3 For test solutions containing more than 1 mg of titanium in the aliquot, add 3,0 ml of sodium
5.11), to prevent the interference of titanium.
trip o lyp ho s p hate s o lutio n (

11 Test report
The test report shall include the following information:
a) a l l i n formation ne ce s s a r y for the identi fic ation o f the s ample, the lab orator y a nd the date o f a na lys i s

or of the test report;

b) me tho d u s e d b y re ference to th i s do c u ment, i . e . I S O 49 42 ;

c) re s u lts and the un it i n wh ich they are expre s s e d;

d) a ny u nu s ua l fe atu re s no te d du ri ng the de term i nation;

e) a ny op eration no t s p e c i fie d i n th i s do c u ment, or any op tiona l op eration wh ich m ight have i n fluence d

the results.

© ISO 2016 – All rights reserved 7

BS ISO 4942:201 6
ISO 4942:2016(E)

Annex A
(informative)
Additional information on the international interlaboratory test

Table 2 was derived from the results of an international trial carried out in 1985 on six steel samples
and one pig iron sample in six countries and involving 11 laboratories.
The results of the trial were reported in the ISO/TC 17/SC 1 N 647, March 1986 document. The precision
data are presented in graphical form in Figure B.1.
The test samples used are listed in Table A.1.
Table A.1 — Test samples used for the precision test

Vanadium content
% (mass fraction)
Sample
Found
Certified
m1 m2
JSS 513–4 0,005 0,004 9 0,004 9
( low- a l loy s te el )

JSS 113–2 0,007 0,007 0 0,007 0

(pig iron)
JSS 516–4 0,010 0,010 2 0,010 6
( low- a l loy s te el )

JSS 652–7 0,038 a 0,038 2 0,038 0

(stainless steel)
JSS 152–8 0,10 0,103 0,103
( low- a l loy s te el )

JSS 153–7 0,21 0,213 0,212

( low- a l loy s te el )

JSS 603–7 0,46 0,456 0,459

(tool steel)
m1 i s the genera l me a n with i n a d ay.

m2 i s the genera l me a n b e twe en d ays .

a N o n- cer ti fie d va lue .

8 © ISO 2016 – All rights reserved

 BS ISO 4942:201 6
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Annex B
(informative)
Graphical representation of precision data

Key
r
Rw
R
X vanadium content (mass fraction)
Y precision (%)
Figure B.1 — Relationship between vanadium content and repeatability limit (r) and
reproducibility limits (Rw and R )

© ISO 2016 – All rights reserved 9

BS ISO 4942:201 6
ISO 4942:2016(E)

Bibliography

[1] ISO 5725:19862) , Precision of test methods — Determination of repeatability and reproducibility
for a standard test method by inter-laboratory tests

2) Withdrawn. (Rep laced by I S O 5 7 2 5 s eries . )

10 © ISO 2016 – All rights reserved

BS ISO 4942:201 6
BS ISO 4942:201 6
ISO 4942:2016(E)

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