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39:1994
ISO 10138:1991
Analytical laboratories
Department of Defence, Australia, Materials Research Laboratory
Steel manufacturers
STANDARDS AUSTRALIA
1 The Crescent,
Homebush NSW 2140 Australia
STANDARDS NEW ZEALAND
Level 10, Standards House,
155 The Terrace,
Wellington 6001 New Zealand
ISBN 0 7262 8900 0
ii
PREFACE
This Standard was prepared by the Joint Standards Australia/Standards New Zealand Committee
CH/10 on the Analysis of Metals.
This Standard is issued as a Joint Standard under the terms of the Active Cooperation Agreement
between Standards Australia and Standards New Zealand.
This Standard is technically identical to ISO 10138:1991, Steel and iron —Determination of
chromium content — Flame atomic absorption spectrometric method published by the International
Organization for Standardization (ISO). This ISO Standard was drafted with input by
Committee CH/10.
This Standard specifies flame atomic absorption spectrometric method for the determination of
chromium content between 0.002% (m/m) and 2.0% (m/m) in non-alloy and low-alloy steel. The
This is a free 7 page sample. Access the full version at http://infostore.saiglobal.com.
procedure involves dissolution of a test portion in acid, oxidation and removal of silica. The
remaining material is fused, extracted, then added to the reserved filtrate. This solution is then
delivered to a dinitrogen monoxide-acetylene flame for spectrometric measurement of the atomic
absorption of the 357.9 nm or 425.4 nm spectral line emitted by a chromium hollow cathode lamp.
Under arrangements made between Standards Australia/Standards New Zealand and the international
Standards bodies, ISO and IEC, as well as certain other Standards organizations, users of this
Standard are advised that the number of this Standard is not reproduced on each page. Its identity is
shown only on the cover and title pages.
The terms ‘normative’ and ‘informative’ have been used in this Standard to define the application of
the annex to which they apply. A ‘normative’ annex is an integral part of a Standard, whereas an
‘informative’ annex is only for information and guidance.
For the purpose of this Standard, the ISO text should be modified as follows:
(a) Terminology The words ‘Australian Standard’, ‘New Zealand Standard’ or ‘Joint
Australian/New Zealand Standard’ should replace the words ‘International Standard’ wherever
they appear.
(b) References The references to International Standards should be replaced by references to the
following Australian/New Zealand Standards:
Reference to International Standard Australian/New Zealand Standard
ISO AS
377 Selection and preparation of samples and 1213 Iron and steel—Methods of sampling
test pieces of wrought steels
377.2 Part 2: Samples for the determination
of the chemical composition
385 Laboratory glassware—Burettes 2165 Burettes and bulb burettes
385.1 Part 1: General requirements
648 La b or a to r y g la s sw a r e — O n e - m ar k 2166 One-mark pipettes
pipettes
1042 Laboratory glassware —One-mark volu- 2164 One-mark volumetric flasks
metric flasks
3696 W ater f or ana lytical labor a tor y —
use —Specification and test methods
5725 Precision of test methods — Deter- 2850 Chemical analysis—Interlaboratory test
minati on of r e peatabil ity and programs—For determining precision of
reproducibility for a standard test analytical method(s)—Guide to the
method by inter-laboratory tests planning and conduct
iii
CONTENTS
Page
1 SCOPE . . . . . . . . . . . . . . . . . .. .. .. .. . . .. .. .. . .. .. . .. ......... 1
2 NORMATIVE DOCUMENTS . . .. .... .. . . .... .. . .. .. . .. ......... 1
3 PRINCIPLE . . . . . . . . . . . . . . .. .... .. . . .... .. . .. .. . .. ......... 1
4 REAGENTS . . . . . . . . . . . . . .. .... .. . . .... .. . .. .. . .. . .. ... .. . 1
5 APPARATUS . . . . . . . . . . . . .. .... .. . . .... .. . .. .. . .. .. .. ... .. 2
6 SAMPLING . . . . . . . . . . . . . . .. .... .. . . .... .. . .. .. . .. .. ... .. .. 3
7 PROCEDURE . . . . . . . . . . . . .. .... .. . . .... .. . .. .. . .. .. .. ... .. 3
8 EXPRESSION OF RESULTS . .. .... .. . . .... .. . .. .. . .. .......... 5
9 TEST REPORT . . . . . . . . . . . .. .... .. . . .... .. . .. .. . .. . .. .. ... .. 6
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ANNEXES
A PROCEDURES FOR THE DETERMINATION OF INSTRUMENTAL
CRITERIA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
B ADDITIONAL INFORMATION ON THE INTERNATION
CO-OPERATIVE TESTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
C GRAPHICAL REPRESENTATION OF PRECISION DATA . . . . . . . . . . . 10
iv
NOTES
1
Part 39:
Determination of chromium content—Flame
atomic absorption spectrometric method
1 Scope 3 Principle
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This International Standard specifies a flame atomic Dissolution of a test portion in hydrochloric acid,
absorption spectrometric method for the determi- followed by oxidation with nitric acid.
nation of chromium in non-alloy and low-alloy steels
and iron.
Filtration and ignition of the acid insoluble residue.
Removal of silica with hydrofluoric acid.
The method is applicable to chromium contents
between 0,002 % (m/m) and 2,0 % (m/m).
Fusion of the residue with potassium hydrogen
sulfate, extraction of the melt in acid and addition of
the extract to the reserved filtrate.
2 Normative references
Spraying the solution into a dinitrogen monoxide
The following standards contain provisions which, acetylene flame.
through reference in this text, constitute provisions
of this International Standard. At the time of publi- Spectrometric measurement of the atomic absorption
cation, the editions indicated were valid. All stand- of the 357,9 nm or 425,4 nm spectral line emitted by
ards are subject to revision, and parties to a chromium hollow cathode lamp.
agreements based on this International Standard are
encouraged to investigate the possibility of applying
the most recent editions of the standards indicated
below. Members of IEC and ISO maintain registers of 4 Reagents
currently valid International Standards.
During the analysis, unless otherwise stated, use
ISO 377-2:1989, Selection and preparation of only reagents of recognized analytical grade and only
samples and test pieces of wrought steels — Part 2: grade 2 water as specified in ISO 3696.
Samples for the determination of the chemical
composition. 4.1 Pure iron, containing less than 0,0002 % (m/m)
chromium
ISO 385-1:1984, Laboratory glassware — Burettes —
Part 1: General requirements.
4.2 Potassium hydrogen sulfate (KHS O4 ).
ISO 648:1977, Laboratory glassware — One-mark
pipettes. 4.3 Hydrochloric acid, ρ about 1,19 g/ml.
ISO 1042:1983, Laboratory glassware — One-mark 4.4 Nitric acid, ρ about 1,40 g/ml.
volumetric flasks.
ISO 3696:1987, Water for analytical laboratory use — 4.5 Hydrofluoric acid, ρ about 1,15 g/ml.
Specification and test methods.
4.6 Sulfuric acid, ρ about 1,84 g/ml.
ISO 5725:1986, Precision of test methods —
Determination of repeatability and reproducibility for a
4.7 Sulfuric acid, ρ about 1,84 g/ml, diluted 1 + 3.
standard test method by inter-laboratory tests.
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