BRITISH STANDARD BS EN

12441-1:2002
Incorporating
Amendment No. 1

Zinc and zinc alloys —

Chemical analysis —
Part 1: Determination of aluminium in
zinc alloys — Titrimetric method

The European Standard EN 12441-1:2001, with the incorporation of

amendment A1:2004, has the status of a British Standard

ICS 77.120.60; 77.040.30

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BS EN 12441-1:2002

National foreword
This British Standard is the official English language version of
EN 12441-1:2001, including amendment A1:2004. It supersedes
BS 3630-6:1965 which is withdrawn.
The UK participation in its preparation was entrusted by Technical Committee
NFE/8, Zinc and zinc alloys, to Subcommittee NFE/8/4, Sampling and analysis
of zinc and zinc alloys, which has the responsibility to:
— 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 international and European developments and
promulgate them in the UK.
A list of organizations represented on this subcommittee 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 “International 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 its correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, the EN title page,
pages 2 to 10, an inside back cover and a back cover.
The BSI copyright notice displayed in this document indicates when the
document was last issued.
This British Standard, having
been prepared under the
direction of the Engineering
Sector Policy and Strategy
Committee, was published Amendments issued since publication
under the authority of the
Standards Policy and Strategy Amd. No. Date Comments
Committee on 23 January 2002

© BSI 26 August 2004 15354 26 August 2004 Changes to Table 1

ISBN 0 580 38161 7

EUROPEAN STANDARD EN 12441-1
NORME EUROPÉENNE October 2001

EUROPÄISCHE NORM + A1
August 2004

ICS 77.040.30; 77.1 20.60

English version

Zinc and zinc alloys - Chemical analysis - Part 1 : Determination

of aluminium in zinc alloys - Titrimetric method
(includes amendment A1 :2004)

Zinc et alliages de zinc - Analyse chimique - Partie 1 : Zink und Zinklegierungen - Chemische Analyse - Teil 1 :
Dosage de l'aluminium dans les alliages de zinc - Méthode Bestimmung von Aluminium in Zinklegierungen -
titrimétrique Titrimetrisches Verfahren
(inclut l’amendement A1 :2004) (enthält Änderung A1 :2004)

This European Standard was approved by CEN on 1 1 August 2001 , and amendment A1 was approved by CEN on 21 June 2004.
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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

C O MITÉ EURO P ÉEN D E NO RMALIS ATIO N
E U RO P Ä I S C H E S KO M I T E E F Ü R N O RM U N G

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

© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 1 2441 -1 :2001 + A1 :2004 E
worldwide for CEN national Members.
EN 1 2441 -1 :2001 (E)

Contents
page
Foreword...................................................................................................................................................................... 3
1 Scope .............................................................................................................................................................. 5
2 Normative references .................................................................................................................................... 5
3 Terms and definitions ................................................................................................................................... 5
4 Principle .......................................................................................................................................................... 5
5 Reagents ......................................................................................................................................................... 5
6 Apparatus ....................................................................................................................................................... 6
7 Sampling ......................................................................................................................................................... 6
8 Procedure ....................................................................................................................................................... 6
9 Calculation and expression of results......................................................................................................... 7
10 Test report ...................................................................................................................................................... 8
Annex A (i n form ati ve) Additional information on round - Robin tests .................................................................. 9
Annex B (i n form ati ve) Graphical representation of precision data ..................................................................... 1 0

2
 EN 1 2441 -1 :2001 (E)

Foreword
Th i s E u ro p e a n S ta n d a rd h as been p re p a re d by T e ch n i ca l C o m m i tte e C E N /T C 209, " Zi n c and zi n c a l l o ys " , th e

s e cre ta ri a t o f wh i ch is hel d b y AF N O R.

Th i s E u ro p e a n S ta n d a rd sh al l be g i ve n th e s ta tu s of a n a ti o n a l s ta n d a rd , e i th e r b y p u b l i ca ti o n of an i d e n ti ca l te xt o r

by e n d o rs e m e n t, at th e l a te s t by Ap ri l 2 002, an d co n fl i cti n g n a ti o n a l s ta n d a rd s s h al l be wi th d ra wn at th e l a te s t by

Ap ri l 2 002 .

W i th i n i ts p ro g ra m m e of wo rk, T e ch n i ca l C o m m i tte e C E N /T C 209 e n tru s te d C E N /T C 2 0 9 /W G 6 “ M e th o d s of

a n a l ys i s an d te s ti n g ” wi th th e p re p a ra ti o n o f th e fo l l o wi n g d o cu m e n t:

EN Zinc and zinc alloys - Chemical analysis - Part 1: Determination of aluminium in zinc alloys –
1 2 4 4 1 -1 ,

Titrimetric method .

Th i s s ta n d a rd is p a rt o f a s e ri e s o f e l e ve n s ta n d a rd s . Th e o th e r s ta n d a rd s a re :

 Part 2 : Determination of magnesium in zinc alloys – Flame atomic absorption spectrometric method
 Part 3 : Determination of lead, cadmium and copper - Flame atomic absorption spectrometric method
 Part 4 : Determination of iron in zinc alloys - Spectrophotometric method
 Part 5 : Determination of iron in primary zinc - Spectrophotometric method
 Part 6 : Determination of aluminium and iron - Flame atomic absorption spectrometric method
 Part 7 : Determination of tin - Flame atomic absorption spectrometric method after extraction
 Part 8 : Determination of tin in secondary zinc - Flame atomic absorption spectrometric method
 Part 9 : Determination of nickel in zinc alloys - Flame atomic absorption spectrometric method
 Part 10 : Determination of chromium and titanium in zinc alloys – Spectrophotometric method
 Part 11 : Determination of silicon in zinc alloys - Spectrophotometric method
Th e a n n e xe s A an d B a re i n fo rm a ti ve .

Acco rd i n g to th e C E N /C E N E L E C I n te rn a l Re g u l a ti o n s , th e n a ti o n a l s ta n d a rd s o rg a n i za ti o n s of th e fo l l o wi n g

co u n tri e s a re bou n d to i m pl em en t th i s E u ro p e a n S ta n d a rd : Au s tri a , Bel g i u m , C ze ch Re p u b l i c, D e n m a rk, Fin lan d,

F ra n ce , G e rm a n y, G re e ce , I ce l a n d , I re l a n d , I ta l y, Lu xem b o u rg , N e th e rl a n d s , N o rwa y, P o rtu g a l , Spai n , S we d e n ,

S wi tze rl a n d and th e U n i te d Ki n g d o m .

3
EN 1 2441 -1 :2001 (E)

Foreword to amendment A1
Th i s d ocu m en t (EN 1 2 441 -1 : 2001 /A1 : 2 004) h as been prepared b y Tech n i cal Com m i ttee CEN /TC 209, "Zi n c an d
zi n c al l oys ", th e secretari at of wh i ch i s h el d b y AFN OR.

Th i s Am en d m en t to th eE u ropean Stan d ard sh al l be g i ven th e statu s of a n ati on al stan d ard , ei th er by pu bl i cati on of

an i d en ti cal text or by en d orsem en t, at th e l atest b y Febru ary 2 005, an d con fl i cti n g n ati on al stan d ard s sh al l be
wi th d rawn at th e l atest by Febru aryl 2005 .

Accord i n g to th e CEN /CE N ELEC I n tern al Reg u l ati on s, th e n ati on al stan d ard s org an i zati on s of th e fol l owi n g
cou n tri es are bou n d to i m pl em en t th i s Eu ropean Stan d ard : Au stri a, Bel g i u m , Cypru s, Czech Repu bl i c, D en m ark,
Eston i a, Fi n l an d , Fran ce, G erm an y, G reece, H u n g ary, I cel an d , I rel an d , I tal y, Latvi a, Li th u an i a, Lu xem bou rg , M al ta,
N eth erl an d s, N orway, Pol an d , Portu g al , Slovaki a, Sl oven i a, S pai n , Swed en , Swi tzerl an d an d U n i ted Ki n g d om .

4
 EN 1 2441 -1 :2001 (E)

1 Scope
Th i s Eu ropean Stan d ard speci fi es a ti tri m etri c m ethod for th e d eterm i n ati on of al u m i n i u m i n zi n c al l oys. I t is
appl i cabl e to th e prod u cts speci fi ed i n EN 1 774 an d EN 1 2844.

I t i s su i tabl e for th e d eterm i n ati on of al u m i n i u m con ten ts (m ass fracti on s) between 3 % an d 30 %.

2 Normative references
Th i s Eu ropean Stan d ard i n corporates b y d ated or u n d ated referen ce, provi si on s from oth er pu bl i cati on s. Th ese
n orm ati ve referen ces are ci ted at th e appropri ate pl aces i n th e text, an d th e pu bl i cati on s are l i sted h ereafter. For
d ated referen ces, su bseq u en t am en d m en ts to or revi si on s of an y of th ese pu bl i cati on s appl y to th i s Eu ropean
Stan d ard on l y wh en i n corporated i n i t by am en d m en t or revi si on . For u n d ated referen ces, th e l atest ed i ti on of th e
pu bl i cati on referred to appl i es (i n cl u d i n g am en d m en ts). 5

EN 1 774, Zinc and zinc alloys - Alloys for foundry purposes - Ingot and liquid.
EN 1 2060, Zinc and zinc alloys - Method of sampling - Specifications.
EN 1 2844, Zinc and zinc alloys - Castings - Specifications.
I SO 5725-1 , Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles
and definitions.

3 Terms and definitions

For th e pu rposes of th i s Eu ropean Stan d ard , th e term s an d d efi n i ti on s g i ven i n EN 1 2060 appl y.

4 Principle
An excess of EDTA i s ad d ed to th e h yd roch l ori c sol u ti on of a test porti on . Th i s i s fol l owed b y q u an ti tati ve
com pl exi n g of th e excess wi th a stan d ard zi n c sol u ti on . Th e al u m i n i u m -EDTA com pl ex i s d ecom posed wi th sod i u m
fl u ori d e an d th e l i berated E DTA i s ti trated ag ai n st a stan d ard zi n c sol u ti on .

5 Reagents
5.1 General
Du ri n g th e test, u se on l y reag en ts of kn own an al yti cal g rad e an d d i sti l l ed or d em in eral i zed water.

5.2 Hydrochloric acid , ρ = 1 , 1 9 g /m l

5.3 Nitric acid , ρ = 1 , 4 g /m l
5.4 Hydrochloric acid (1 + 1)

M i x 1 vol u m e of h yd roch l ori c aci d (5. 2) wi th 1 vol u m e of water.

5.5 Hydrogen peroxide , 30 % (m ass fracti on )

5.6 Hydroxylammonium chloride, 200 g /l sol u ti on

5.7 Ethylenediamine tetra-acetic acid disodium salt (EDTA) , 65 g /l sol u ti on

5
EN 1 2441 -1 :2001 (E)

5.8 Ammonia solution, ρ = 0, 91 g /m l

5.9 Sodium fluoride , satu rated sol u ti on

Di ssol ve 60 g of sod i u m fl u ori d e i n 1 l of boi l i n g water. Cool to room tem peratu re an d fi l ter.

5.1 0 Sodium acetate, bu ffer sol u ti on

Di ssol ve 1 35 g of sod i u m acetate (CH COON a, 3H O) i n approxi m atel y 300 m l of water. Ad d 1 3 m l of g l aci al aceti c
3 2

aci d (5. 1 6). Ch eck th at th e pH i s wi th i n th e ran g e 5 to 5, 5. M ake u p th e vol u m e to 500 m l wi th water.

5.1 1 Standard zinc solution , 0, 05 M

Di ssol ve 3, 2 69 g of h i g h pu ri ty zi n c i n 40 m l of h yd roch l ori c aci d (1 + 1 ) (5. 4) i n a 2 50 m l beaker fi tted wi th a
watch -g l ass. Di l u te wi th 1 00 m l of water. Ad d 2 d rops of m eth yl red sol u ti on (5. 1 2). N eu tral i ze wi th am m on i a
sol u ti on (5. 8). Ad d h yd roch l ori c aci d (1 +1 ) (5. 4) d rop by d rop u n ti l th e col ou r ch an g es to red . Tran sfer q u an ti tati vel y
to a 1 l vol u m etri c fl ask. Ad d 5 m l of h yd roch l ori c aci d (1 + 1 ) (5. 4), d i l u te to th e m ark wi th water an d m i x.

1 m l of th i s sol u ti on correspon d s to 1 , 349 m g of al u m i n i u m .

5.1 2 Methyl red , eth an ol i c sol u ti on

Di ssol ve 0, 02 g of m eth yl red i n 1 00 m l of eth an ol .

5.1 3 Xylenol orange , 1 0 g /l sol u ti on

5.1 4 Aqua regia
M i x 3 vol u m es of h yd roch l ori c aci d (5. 2) wi th 1 vol u m e of n i tri c aci d (5. 3).

5.1 5 Xylene cyanol , 1 g /l sol u ti on .

N OTE U se of th is reag en t i s opti onal .

5.1 6 Glacial acetic acid , ρ = 1 , 05 g /m l

6 Apparatus
Al l g l assware u sed for th e preparati on of th e sol u ti on s an d for th e i m pl em en tati on of th e m eth od sh al l be cl ean ed
wi th boi l i n g aq u a reg i a (5. 1 4) pri or to u se.

7 Sampling
Th e test sam pl e sh al l be sel ected an d prepared i n accord an ce wi th th e proced u re g i ven i n EN 1 2 060.

8 Procedure
8.1 Test portion
Wei g h , 5 g of th e test sam pl e to th e n earest 0, 001 g .

8.2 Determination
8.2.1 I n trod u ce th e test porti on (8. 1 ) i n to a 500 m l beaker fi tted wi th a watch -g l ass an d d i ssol ve by carefu l l y
ad d i n g 50 m l of h yd roch l ori c aci d (1 + 1 ) (5. 4). Oxi d i ze an d com pl ete th e d i ssol u ti on b y ad d i n g a few d rops of
h yd rog en peroxi d e (5. 5).

6
 EN 1 2441 -1 :2001 (E)

8.2.2 Ad d 5 m l of h yd roxyl am m on i u m ch l ori d e sol u ti on (5. 6) to d ecom pose th e excess of h yd rog en peroxi d e.
H eat th e beaker carefu l l y.

Di l u te to 1 00 m l wi th water an d cool to room tem peratu re. Tran sfer q u an ti tati vel y:

a) for Al con ten ts (m ass fraction s) ≤ 1 5 % : to a 250 m l vol u m etri c fl ask ;

b) for Al con ten ts (m ass fraction s) ≥ 1 5 % : to a 1 000 m l vol u m etri c fl ask.

Di l u te to th e m ark wi th water an d m i x.

8.2.3 Tran sfer a 25 m l al i q u ot to a 500 m l con i cal fl ask.

8.2.4 Ad d su ccessi vel y :

a) approxi m atel y 1 00 m l of water;

b)

1) for Al con ten ts (m ass fraction s) ≤ 1 5 % : 55 m l of EDTA sol u ti on (5. 7) ;

2) for Al con ten ts (m ass fraction s) ≥ 1 5 % : 25 m l of EDTA sol u ti on (5. 7).

c) 5 d rops of m eth yl red sol u ti on (5. 1 2).

8.2.5 N eu tral i ze exactl y wi th am m on i a sol u ti on (5. 8) u n ti l th e col ou r ch an g es to yel l ow. Ad d 25 m l of bu ffer

sol u ti on (5. 1 0).

8.2.6 Boi l for 2 to 3 m i n . Cool to room tem peratu re.

8.2.7 Ad d 2 to 3 d rops of xyl en ol oran g e sol u ti on (5. 1 3).

N OTE For som e operators th e en d -poi n t can be mad e even m ore read il y d etectabl e by the ad d i tion of not more than 1 ml
of xyl en e cyan ol solu ti on (5. 1 5).

8.2.8 Ti trate th e excess of EDTA wi th stan d ard zi n c sol u ti on (5. 1 1 ) u n ti l th e col ou r ch an g es to pu rpl e.

8.2.9 Ad d 25 m l of sod i u m fl u ori d e sol u ti on (5. 9). B oi l for 2 to 3 m i n u tes. Cool to room tem peratu re.

8.3 Volumetric measurement

Ti trate th e l i berated EDTA wi th th e stan d ard zi n c sol u ti on (5. 1 1 ) u n ti l th e col ou r ch an g es to pu rpl e.

9 Calculation and expression of results

9.1 Method of calculation
Th e al u m i n i u m con ten t sh al l be g i ven , as a percen tag e by m ass,

a) for Al con ten ts (m ass fraction s) ≤ 1 5 % : b y th e form u l a V x 0, 269 8 ;

b) for Al con ten ts (m ass fraction s) ≥ 1 5 % : b y th e form u l a V x 1 , 079 2,

wh ere V i s th e vol u m e, i n m i l l i l i tres, of stan d ard zi n c s ol u ti on u sed to ti trate th e l i berated EDTA (see 8. 3).

I f a n u m ber of d eterm i n ati on s are carri ed ou t, th en th e m ean of al l th e resu l ts sh al l be cal cu l ated by ad d i n g th e

i n d i vi d u al resu l ts an d d i vi d i n g b y th e n u m ber of i n d i vi d u al resu l ts.

Th e resu l ts sh al l be expressed as speci fi ed i n E N 1 774 an d EN 1 2 844.

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EN 1 2441 -1 :2001 (E)

9.2 Precision
Repeatabi l i ty an d reprod u cti bi l i ty l i m i ts are g i ven i n Tabl e 1 .

N OTE Tabl e 1 has been establi sh ed accord i n g to an nex A. Graph i cal represen tati on of preci sion d ata i s g i ven i n an n ex B.

Table 1 — Repeatability and reproducibility limits

Aluminium content Repeatability limit Reproducibility limit

% r Rw R

2 0, 028 0, 025 0, 050

5 0, 050 0, 050 0, 1 02

10 0, 078 0, 085 0, 1 75

20 0, 1 20 0, 1 43 0, 300

30 0, 1 55 0, 1 95 0, 41 0

1 0 Test report
Th e test report sh al l i n cl u d e th e fol l owi n g :

a) i d en ti fi cati on of th e sam pl e ;

b) test m eth od u sed , (i . e. referen ce to th i s stan d ard ) ;

c) al u m i n i u m con ten t, expressed as percen tag e by m ass, g i vi n g wh ere possi bl e th e resu l ts for th e i n d i vi d u al an d
m ean val u es ;

d) an y u n u su al occu rren ce d u ri n g th e d eterm i n ati on ;

e) an y steps i n th e proced u re be yon d th ose speci fi ed i n th i s stan d ard , an d an y ci rcu m stan ces th at m ay h ave
affected th e resu l ts ;

f) d ate of testi n g ;

g) n am e of l aboratory or testi n g org an i zati on ;

h) si g n atu re of th e l aboratory m an ag er or oth er respon si bl e person .

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 EN 1 2441 -1 :2001 (E)

Annex A
(i n form ati ve)

Additional information on round - Robin tests

Tabl e 1 was d eri ved from th e resu l ts of Eu ropean an al yti cal tri al s carri ed ou t i n 1 998 i n 6 cou n tri es i n vol vi n g 1 3
l aboratori es, u si n g 7 sam pl es wi th 5 l evel s of al u m i n i u m con ten ts, each l aboratory m aki n g th ree d eterm i n ati on s of
al u m i n i u m con ten t i n each sam pl e (see n otes 1 an d 2).

Th e resu l ts of th e tri al s were reported i n th e d ocu m en t CEN /TC 209/WG 6 N 69. Th e d etai l s of th e sam pl es u sed
are g i ven i n th e Tabl e A. 1 .

N OTE 1 Two of th e th ree d etermi n ati on s were carried ou t u nd er repeatabi l i ty con d i ti on s as d efi ned i n I SO 5725-1 ; i . e. on e
operator, same apparatu s, i d en ti cal operati n g con d i ti on s and a m in im u m period of ti m e.

N OTE 2 Th e th i rd d etermi n ati on was carri ed ou t on a d i fferen t d ay by th e sam e operator as i n n ote 1 , u si n g th e same
apparatu s.

Th e resu l ts obtai n ed were treated stati sti cal l y i n accord an ce wi th I SO 572 5-1 .

Th e d ata obtai n ed sh owed a l og ari th m i c rel ati on sh i p between th e al u m i n i u m con ten t an d th e repeatabi l i ty ( r) an d
reprod u ci bi l i ty l i m i ts (R an d R) of th e test resu l ts (see n ote 3), as su m m ari sed in Tabl e 1. Th e g raph i cal
w

represen tati on of th e d ata i s sh own i n Fi g u re B. 1 .

N OTE 3 From th e two val u es obtai n ed i n d ay 1 , th e repeatabi l i ty ( r) an d th e reprod u ci bi l i ty l im i t ( R) were cal cu l ated u sin g the

proced u re speci fi ed in I SO 5725-1 . From the fi rst val u e obtai n ed i n d ay 1 an d the valu e obtai n ed i n d ay 2, th e wi th i n -l aboratory
reprod u ci bi li ty l im i t ( R ) was cal cu l ated u si ng th e proced u re speci fi ed in I SO 5725-1 .
w

Table A.1 — Chemical composition in percent of test samples used in the round - Robin test
Sam pl e Al Cu Mg Fe Pb Sn Cd Ni Si

ZL2 4, 00 2, 9 0, 037 0, 006 0, 002 < 0, 001 < 0, 001 < 0, 001 < 0, 02

ZL3 4, 00 < 0, 01 0, 035 0, 002 0, 002 < 0, 001 < 0, 001 < 0, 001 < 0, 02

ZL5 3, 97 0, 8 0, 036 0, 003 0, 002 < 0, 001 < 0, 001 < 0, 001 < 0, 02

ZL6 5, 75 1 ,3 < 0, 000 5 0, 006 0, 002 < 0, 001 < 0, 001 - < 0, 02

ZL8 8, 37 1 ,1 0, 021 0, 003 0, 003 < 0, 001 < 0, 001 < 0, 001 < 0, 02

ZL1 2 1 1 , 00 0, 8 0, 023 0, 01 0, 002 < 0, 001 < 0, 001 - < 0, 02

ZL27 26, 83 2, 3 0, 01 2 0, 04 0, 002 < 0, 001 < 0, 001 - < 0, 02

9
EN 1 2441 -1 :2001 (E)

Annex B
(i n form ati ve)

Graphical representation of precision data

Fi g u re B. 1 i n d i cates th e l og ari th m i c rel ati on sh i ps between al u m i n i u m con ten t an d th e repeatabi l i ty ( r) an d

reprod u ci bi l i ty l i m i ts ( R an d R).
w

l og r= 0, 633 6 × l og WAI - 1 , 744 4

l og Rw = 0, 757 4 × l og WAI - 1 , 829 9

l og R = 0, 774 6 × l og WAI - 1 , 531 0

wh ere WAI i s th e averag e al u m i n i u m con ten t, expressed as a percen tag e b y m ass, obtai n ed from th e th ree

d eterm i n ati on s i n each l aboratory

Key
A Precisi on i n percen t

B Al u m i n i u m con ten t in percen t

Figure B.1 — Logarithmic relationship between aluminium content and the repeatability ( r) and
reproducibility limits (Rw and R)

10
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BS EN
12441-1:2002
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