ISO 11437:2018
(Main)Nickel alloys — Determination of lead — Electrothermal atomic absorption spectrometric method
Nickel alloys — Determination of lead — Electrothermal atomic absorption spectrometric method
ISO 11437:2018 specifies an electrothermal atomic absorption spectrometric method for the determination of lead in the range of 1 µg/g to 10 µg/g in nickel alloys.
Alliages de nickel — Détermination du plomb — Méthode par spectrométrie d'absorption atomique électrothermique
General Information
Relations
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 11437
First edition
2018-01
Nickel alloys — Determination of lead
— Electrothermal atomic absorption
spectrometric method
Alliages de nickel — Détermination du plomb — Méthode par
spectrométrie d'absorption atomique électrothermique
Reference number
©
ISO 2018
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of 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 of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Instrument criteria . 3
7.1 Preparation of solutions required for testing criteria . 3
7.2 Characteristic mass . 3
7.3 Minimum precision . 3
7.4 Limit of detection . 3
7.5 Linearity . . 4
8 Sampling and sample preparation . 4
9 Procedure. 4
9.1 Preparation of the test solution . 4
9.2 Blank test . 4
9.3 Preparation of the calibration solutions . 4
9.4 Calibration and determination . 4
9.4.1 Adjustment of the atomic absorption spectrometer. 4
9.4.2 Atomic absorption measurements . 5
9.5 Number of determinations . 5
10 Expression of results . 6
10.1 Calculation . 6
10.2 Precision . 6
10.2.1 Interlaboratory tests . 6
10.2.2 Precision data . 6
11 Test report . 7
Annex A (normative) Optimization and checking of spectrometer performance criteria .8
Bibliography .15
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. 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 of
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
different types of ISO documents should be noted. This document was drafted 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 of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of 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 information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity 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.
This document was prepared by Technical Committee ISO/TC 155, Nickel and nickel alloys.
This first edition cancels and replaces ISO 11437-1:1994 and ISO 11437-2:1994, which have been merged
and technically revised.
iv © ISO 2018 – All rights reserved
INTERNATIONAL STANDARD ISO 11437:2018(E)
Nickel alloys — Determination of lead — Electrothermal
atomic absorption spectrometric method
1 Scope
This document specifies an electrothermal atomic absorption spectrometric method for the
determination of lead in the range of 1 µg/g to 10 µg/g in nickel alloys.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
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 in a mixture of nitric acid and hydrofluoric acid, dilution of the test solution
to a known volume, and transfer of an aliquot to a plastic vial.
Addition of a modifier to the aliquot of the test solution, and injection of a small volume of this solution
into the electrothermal atomizer of an atomic absorption spectrometer.
Measurement of the atomic absorption of the 283,3 nm spectral line energy emitted by a lead hollow-
cathode lamp and comparison with those of the calibration solutions.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity.
5.1 Pure nickel, containing less than 1 µg/g of lead.
5.2 Nickel, base-solution 50 g/l.
Weigh, to the nearest 0,1 g, 25,0 g of pure nickel (5.1). Transfer to a 600 ml tall-form beaker and add
100 ml of water. Cautiously add 100 ml of nitric acid (ρ = 1,41 g/ml) in small portions, in such a
manner that the dissolution remains under control. Cool the solution and transfer it to a 500 ml one-
mark volumetric flask. Make up to the mark with water and mix.
If large nickel turnings or chunks are used, gentle heating may be required to complete the dissolution.
When using carbonyl nickel powder, the solution should be filtered to remove undissolved carbon.
5.3 Nickel, base solution 5 g/l.
Transfer 10,0 ml of the nickel base solution (5.2) to a 100 ml one-mark volumetric flask. Make up to the
mark with water and mix.
5.4 Nitric acid, ρ = 1,41 g/ml, diluted 1 + 1.
5.5 Hydrofluoric acid, ρ = 1,13 g/ml.
WARNING — Hydrofluoric acid is extremely irritating and corrosive to skin and mucous
membranes producing severe skin burns which are slow to heal. In case of contact with skin,
wash well with water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate and
seek immediate medical treatment.
5.6 Nitric/hydrofluoric acids, mixture.
Carefully add 150 ml of nitric acid (ρ = 1,41 g/ml) and 150 ml of hydrofluoric acid (5.5) to 150 ml of
water. Mix and store in a plastic bottle.
5.7 Modifier, nickel nitrate-ammonium phosphate solution.
Weigh, to the nearest 0,1 g, 6,0 g of ammonium dihydrogen orthophosphate (NH H PO ) and dissolve it
4 2 4
in 50 ml of water. Transfer the solution to a 100 ml one-mark volumetric flask. Add 20,0 ml of the nickel
base solution (5.2), make up to the mark with water and mix.
This solution shall be freshly prepared.
5.8 Lead, standard solution, 100 mg/l.
Weigh, to the nearest 0,001 g, 0,100 g of lead of a mass fraction of 99,9 % minimum purity and transfer
to a 250 ml beaker. Add 40 ml of nitric acid (5.6) and heat to assist dissolution. Cool the solution and
transfer it to a 1 000 ml one-mark volumetric flask. Make up to the mark with water and mix.
Store in a polyethylene bottle.
1 ml of this solution contains 0,1 mg of lead.
5.9 Lead, standard solution, 1 mg/l.
Transfer 10,0 ml of the lead standard solution (5.8) into a 1 000 ml one-mark volumetric flask. Add
20 ml of nitric acid (ρ = 1,41 g/ml). Make up to the mark with water and mix.
1 ml of this solution contains 1 µg of lead.
This solution shall be freshly prepared.
6 Apparatus
All volumetric glassware shall be class A and calibrated, in accordance with ISO 648 or ISO 1042 as
appropriate.
Before use, all glassware shall be cleaned by boiling with hydrochloric acid to remove any chemical
contamination.
6.1 Polytetrafluoroethylene (PTFE) beakers, of capacity 100 ml.
2 © ISO 2018 – All rights reserved
6.2 Plastic vials, of capacity 5 ml.
6.3 Plastic volumetric flasks, of capacities 50 ml and 100 ml.
6.4 Micropipettes, of capacities from 2,0 µl to 100 µl.
6.5 Atomic absorption spectrometer.
The atomic absorption spectrometer to be used shall be fitted with an electrothermal atomizer and
shall meet the performance criteria given in Annex A.
The atomic absorption spectrometer and electrothermal atomiser are satisfactory if, after optimization
according to Annex A (A.3 to A.6), they meet the criteria specified in 7.1.
The spectrometer shall be equipped with a background corrector and a fast recording system capable
of measuring peak heights and peak areas. The electrother
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.