BRITISH STANDARD BS EN

12441-5:2003

Zinc and zinc alloys —

Chemical analysis —
Part 5: Determination of iron in
primary zinc — Spectrophotometric
method

The European Standard EN 12441-5:2003 has the status of a

British Standard

ICS 77.040.30; 77.120.60

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BS EN 12441-5:2003
This British Standard was
published under the authority
of the Standards Policy and
Strategy Committee on
3 April 2003
© BSI 3 April 2003
ISBN 0 580 41492 2
National foreword
This British Standard is the official English language version of
EN 12441-5:2003. It supersedes BS 3630-5:1963 which is withdrawn.
The UK participation in its preparation was entrusted to Technical Committee
NFE/8, Zinc and zinc alloys, which has the responsibility to:
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Amd. No. Date Comments
EUROPEAN STANDARD EN 1 2441 -5
NORME EUROPÉENNE
EUROPÄISCHE NORM March 2003

ICS 77.040.30; 77.1 20.60

English version

Zinc and zinc alloys - Chemical analysis - Part 5: Determination

of iron in primary zinc - Spectrophotometric method
Zinc et alliages de zinc - Analyse chimique - Partie 5: Zink und Zinklegierungen - Chemische Analyse - Teil 5:
Dosage du fer dans le zinc primaire - Méthode Bestimmung von Eisen in Primärzink -
spectrophotométrique Spektrophotometrisches Verfahren

This European Standard was approved by CEN on 21 November 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,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United
Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

C OMITÉ EURO PÉEN DE NO RMALIS ATIO N
EUROPÄIS CHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36 B-1 050 Brussels

© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 1 2441 -5:2003 E
worldwide for CEN national Members.
EN 1 2441 -5:2003 (E)

Contents
page
Foreword ......................................................................................................................................................................3
1 Scope ..............................................................................................................................................................4
2 Normative references ....................................................................................................................................4
3 Terms and definitions....................................................................................................................................4
4 Principle ..........................................................................................................................................................4
5 Reagents .........................................................................................................................................................4
6 Apparatus .......................................................................................................................................................5
7 Sampling .........................................................................................................................................................5
8 Procedure .......................................................................................................................................................5
9 Calculation and expression of results .........................................................................................................7
10 Test report ......................................................................................................................................................7

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 EN 1 2441 -5:2003 (E)

Foreword

This document (EN 1 2441 -5:2003) has been prepared by Technical Committee CEN /TC 209 "Zinc and zinc
alloys", the secretariat of which is held by AFNOR.
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 September 2003, and conflicting national standards shall be withdrawn at the
latest by September 2003.
Within its programme of work, Technical Committee CEN/TC 209 entrusted CEN/TC 209/WG 6, “Methods of
analysis and testing” with the preparation of the following document:
EN 1 2441 -5, Zinc and zinc alloys - Chemical analysis – Part 5: Determination of iron in primary zinc –
Spectrophotometric method .
This standard is part of series of eleven standards. The other standards are:
 EN 1 2441 -1 , Zinc and zinc alloys – Chemical analysis – Part 1 : Determination of aluminium in zinc alloys –
Titrimetric method ;
 EN 1 2441 -2, Zinc and zinc alloys – Chemical analysis – Part 2: Determination of magnesium in zinc alloys –
Flame atomic absorption spectrometric method ;
 EN 1 2441 -3, Zinc and zinc alloys – Chemical analysis – Part 3: Determination of lead, cadmium and copper –
Flame atomic absorption spectrometric method ;
 EN 1 2441 -4, Zinc and zinc alloys – Chemical analysis – Part 4: Determination of iron in zinc alloys –
Spectrophotometric method. .
 EN 1 2441 -6, Zinc and zinc alloys – Chemical analysis – Part 6: Determination of aluminium and iron – Flame
atomic absorption spectrometric method ;
 prEN 1 2441 -7, Zinc and zinc alloys – Chemical analysis – Part 7: Determination of tin – Flame atomic
absorption spectrometric method after extraction ;
 prEN 1 2441 -8, Zinc and zinc alloys – Chemical analysis – Part 8: Determination of tin in secondary zinc –
Flame atomic absorption spectrometric method ;
 prEN 1 2441 -9, Zinc and zinc alloys – Chemical analysis – Part 9: Determination of nickel in zinc alloys – Flame
atomic absorption spectrometric method ;
 prEN 1 2441 -1 0, Zinc and zinc alloys – Chemical analysis – Part 1 0: Determination of chromium and titanium in
zinc alloys – Spectrophotometric method ;
 prEN 1 2441 -1 1 , Zinc and zinc alloys – Chemical analysis – Part 1 1 : Determination of silicon in zinc alloys –
Spectrophotometric method ;
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, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,
Slovakia, Spain, Sweden, Switzerland and the United Kingdom.

3
EN 1 2441 -5:2003 (E)

1 Scope
This European Standard specifies a spectrophotometric method for the determination of iron in primary zinc. It is
applicable to the products specified in EN 1 1 79.
It is suitable for the determination of iron contents (mass fractions) between 0,001 % and 0,1 %.

2 Normative references
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).
EN 1 1 79, Zinc and zinc alloys - Primary zinc.
EN 1 2060:1 997, Zinc and zinc alloys - Method of sampling – Specifications.

3 Terms and definitions

For the purposes of this European Standard, the terms and definitions given in EN 1 2060:1 997 apply.

4 Principle
Formation of a sulfosalicylic acid ferric complex in an ammoniacal medium. Spectrophotometric measurement of
the yellow colour of the thus formed complex.

5 Reagents
5.1 General
During the test, use only reagents of known analytical grade and distilled or demineralised water.

5.2 Ammonia solution, ρ = 0,91 g/ml.

5.3 Hydrochloric acid, ρ = 1 ,1 9 g/ml.

5.4 Hydrogen peroxide, 30 % (mass fraction).
5.5 Sulfosalicylic acid, 400 g/l solution.

5.6 Nickel chloride solution

Dissolve 2 g of nickel chloride hexahydrate (NiCl 2.6H 2O) in 500 ml of water. Make up to 1 l and mix.

5.7 Standard iron solution A

Weigh 0,250 g of pure iron to the nearest 0,001 g. Add by small fractions approximately 1 0 ml of hydrochloric acid
(5.3). Oxidise by adding a few drops of hydrogen peroxide (5.4). Decompose the excess hydrogen peroxide by
boiling. Cool to room temperature. Transfer quantitatively to a 1 l volumetric flask. Dilute to the mark with water and
mix.
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 EN 1 2441 -5:2003 (E)

1 ml of this solution contains 0,250 mg of iron.

5.8 Standard iron solution B

Transfer exactly 20 ml of standard iron solution A (5.7) to a 1 00 ml volumetric flask. Dilute to the mark with water
and mix.
1 ml of this solution contains 0,050 mg of iron.

5.9 Nitric acid, ρ = 1 ,4 g/ml.

5.1 0 Aqua regia

Mix 3 volumes of hydrochloric acid (5.3) with 1 volume of nitric acid (5.9).

6 Apparatus
6.1 General
All glassware used for the preparation of the solutions and for the implementation of the method shall be cleaned
with boiling aqua regia (5.1 0) prior to use.

6.2 Specific equipment

In addition to standard laboratory apparatus, a spectrophotometer, set at a wavelength of 425 nm and using 1 cm
optical cells shall be used.
NOTE The dilution and aliquot parts defined in this standard only apply if 1 cm cells are used. It is necessary to apply the
appropriate modifications in the case of cells with other dimensions.

7 Sampling
The test sample shall be selected and prepared in accordance with the procedure given in EN 1 2060.

8 Procedure
8.1 Test portion
Weigh 1 0 g of the test sample to the nearest 0,01 g.

8.2 Blank test

Simultaneously with each determination, carry out a blank test using the same quantities of each reagent and
following the same procedure.

8.3 Preparation of the test solution

8.3.1 Introduce the test portion (8.1 ) in a 500 ml beaker fitted with a watch-glass and dissolve by carefully adding
50 ml of hydrochloric acid (5.3). Oxidise and complete the dissolution by adding a few drops of hydrogen peroxide
(5.4).
If dissolution is very difficult, 2 ml of nickel chloride solution (5.6) should be added to expedite the attack.
8.3.2 Decompose the excess hydrogen peroxide by boiling.
5
EN 1 2441 -5:2003 (E)

8.3.3 For iron contents (mass fractions) equal to or greater than 0,01 % proceed as follows (if less than 0,01 %
see 8.3.4):
a) cool to room temperature. Transfer quantitatively to a 250 ml volumetric flask. Dilute to the mark with water
and mix;
b) transfer a 25 ml aliquot to a 1 00 ml volumetric flask;
c) add successively:
1 ) 25 ml of water;
2) 5 ml of sulfosalicylic acid (5.5);
3) ammonia solution (5.2) until the solution becomes yellow, then 20 ml in excess;
d) cool to room temperature. Dilute to the mark with water and mix.
8.3.4 For iron contents (mass fractions) less than 0,01 % proceed as follows:
a) evaporate the test portion until a syrupy consistency is obtained;
b) cool to room temperature;
c) take up with a minimum of water (so as not to exceed 30 ml) and transfer quantitatively to a 1 00 ml volumetric
flask;
d) add successively:
1 ) 5 ml of sulfosalicylic acid solution (5.5);
2) ammonia solution (5.2) until the solution has a yellow colour, then 50 ml in excess;
e) cool to room temperature. Dilute to the mark and mix. Measure the absorbance of the solutions (see 8.5) after
first measuring the calibration graph as in 8.4.

8.4 Calibration graph

NOTE The following is valid for 1 cm cells and for iron contents (mass fractions) of 0 mg, 0,1 0 mg, 0,25 mg, 0,5 mg and
1 ,00 mg of iron corresponding to mass fractions in the test portion of 0 %, 0,01 %, 0,025 % 0,05 % and 0,1 % when using the
procedure specified in 8.3.3 and 0 %, 0,001 % 0,0025 %, 0,005 % and 0,01 % when using the procedure specified in 8.3.4. It is
necessary to apply the appropriate modifications in the case of cells of different dimensions.

8.4.1 Introduce into a series of 1 00 ml volumetric flasks, 0,00 ml, 2,00 ml, 5,00 ml, 1 0,00 ml and 20,00 ml of
standard iron solution B (5.8).
8.4.2 Add successively:
a) 5 ml of sulfosalicylic acid solution (5.5);
b) ammonia solution (5.2) until the solution becomes yellow, then 20 ml in excess.
8.4.3 Cool to room temperature. Dilute to the mark with water and mix.
8.4.4 Measure the absorbance of each solution against the solution with 0,00 ml standard iron solution B, in 1 cm
cells, using the spectrophotometer (6.2) at a wavelength of 425 nm.
8.4.5 Produce a calibration graph by plotting the iron content versus the absorbance readings obtained for each
calibration standard.

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 EN 1 2441 -5:2003 (E)

8.5 Spectrophotometric measurement

Measure the absorbance of the test solution(s) against the blank solution (8.2) in 1 cm cells using the
spectrophotometer (6.2) at a wavelength of 425 nm.

9 Calculation and expression of results

Determine from the measured absorbance of the test solution the associated amount of iron from the calibration
graph (8.4). If a number of determinations are carried out then the mean of all results shall be calculated by adding
the individual results together and dividing by the number of individual results.
Results shall be expressed as specified in EN 1 1 79.

1 0 Test report
The test report shall include the following:
a) type and identification of the sample;
b) test method used, (i.e. reference to this standard);
c) iron content, expressed as percentage by mass, giving where possible the results for the individual and the
mean values;
d) any unusual occurrence during the determination;
e) any steps in the procedure beyond those specified in this standard, and any circumstances that may have
affected the results;
f) date of testing;
g) name of the laboratory or testing organisation;
h) signature of the laboratory manager or other responsible person.

7
BS EN
12441-5:2003
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