EN ISO 14284:2002

SLOVENSKI STANDARD
01-april-2003
-HNORLQåHOH]R9]RUþHQMHLQSULSUDYDY]RUFHY]DXJRWDYOMDQMHNHPLMVNHVHVWDYH
,62
Steel and iron - Sampling and preparation of samples for the determination of chemical
composition (ISO 14284:1996)
Eisen und Stahl - Entnahme und Vorbereitung von Proben für die Bestimmung der
chemischen Zusammensetzung (ISO 14284:1996)
Fontes et aciers - Prélevement et préparation des échantillons pour la détermination de
la composition chimique (ISO 14284:1996)
Ta slovenski standard je istoveten z: EN ISO 14284:2002
ICS:
77.080.01 Železne kovine na splošno Ferrous metals in general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 14284
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2002
ICS 77.080
English version
Steel and iron - Sampling and preparation of samples for the
determination of chemical composition (ISO 14284:1996)
Fontes et aciers - Prélèvement et préparation des Eisen und Stahl - Entnahme und Vorbereitung von Proben
échantillons pour la détermination de la composition für die Bestimmung der chemischen Zusammensetzung
chimique (ISO 14284:1996) (ISO 14284:1996)
This European Standard was approved by CEN on 21 July 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,
Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14284:2002 E
worldwide for CEN national Members.

CORRECTED 2002-11-13
Foreword
The text of ISO 14284:1996 has been prepared by Technical Committee ISO/TC 17 "Steel" of
the International Organization for Standardization (ISO) and has been taken over as EN ISO
14284:2002 by Technical Committee ECISS/TC 20 "Methods of chemical analysis of ferrous
products", the secretariat of which is held by SIS.
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 March 2003, and conflicting national
standards shall be withdrawn at the latest by March 2003.
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, Iceland, Ireland, Italy,
Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the
United Kingdom.
Endorsement notice
The text of ISO 14284:1996 has been approved by CEN as EN ISO 14284:2002 without any
modifications.
NOTE Normative references to International Standards are listed in Annex ZA (normative).
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
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).
NOTE Where an International Publication has been modified by common modifications,
indicated by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 377 1997 Steel and steel products - Location EN ISO 377 1997
and preparation of samples and
test pieces for mechanical testing
INTERNATIONAL
ISO
STANDARD
First edition
1996-07-01
Steel and iron
- Sampling and preparation
of samples for the determination of Chemical
composition
Fon tes et aciers - Pr&vement et pr6paration des echantillons pour
Ia d&ermina tion de Ia composition chimique
Reference number
ISO 14284:1996(E)
ISO 14284:1996(E)
Page
Contents
1 Scope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2 Normative references . . . . . .
3 Definitions . . . . . . . . . . . . . . . . . . . . .*.
4 Requirements for sampling and Sample preparation . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . .
4.1 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.2 Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.3 Selection of a Sample
4.4 Preparation of a Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.5 Safety precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5 Liquid iron for steelmaking and pig-iron production . . . . . . . . . . . . .
5.1 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.2 Spoon sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.3 Probe sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
54 . Preparation of a Sample for analysis
. . . . . .*.
6 Liquid iron for cast iron production
6.1 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.2 Spoon sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
IQ
............................ ........................................
63 . Probe sampling
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
64 . Preparation of a Sample for analysis
. Sampling and Sample preparation for the determination
. . . . . . . . . . . . . . . . . . . . . . . . .*.
of Oxygen, nitrogen and hydrogen
0 ISO 1996
All rights reserved. Unless otherwise specified, no part of this publication may be repro-
duced or utilized in any form or by any means, electronie or mechanical, including photo-
copying and microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 0 Switzerland
Printed in Switzerland
ii
Liquid steel for steel production . 12
................................................................................. 12
7.1 General
................................................................... 12
7.2 Spoon sampling
7.3 Probe sampling . 13
Preparation of a Sample for analysis . 13
7.4
Sampling and Sample preparation for the determination
7.5
............................................................................. 14
of Oxygen
7.6 Sampling and Sample preparation for the determination
of hydrogen . 14
8 Pig-irons . 15
81 . General . 15
82 . Increment sampling . 15
.................................... 16
83 . Preparation of a Sample for analysis
9 Cast-iron products . 17
9.1 General . 17
9.2 Sampling and Sample preparation . 18
IO Steel products . 19
10.1 General . 19
Selection of a preliminary Sample or a Sample for analysis
10.2
from a cast product . 19
Selection of a preliminary Sample or a Sample for analysis
10.3
....................................................... 19
from a wrought product
Preparation of a Sample for analysis . 21
10.4
...................................................... 22
10.5 Sampling of leaded steel
10.6 Sampling and Sample preparation for the determination
..................................... 22
of Oxygen .
Sampling and Sample preparation for the determination
10.7
of hydrogen .
Annexes
Sampling probes for use with liquid iron and steel . . . . . . . . . . . . . . 24
A
B Sampling probes for use with liquid steel
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
for the determination of hydrogen
. . .
Ill
ISO 14284:1996(E]
0 ISO
Foreword
ISO (the International Organization for Standardization) is a worldwide fed-
eration of national Standards bodies (ISO member bodies). The work of
preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established has the right to be rep-
resented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO col-
laborates closely with the International Electrotechnical Commission (IEC)
on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are cir-
culated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 14284 was prepared by Technical Committee
lSO/TC 17, Steel, Subcommittee SC 1, Methods of determination of
Chemical composition.
lt cancels and replaces ISO 377-2:1989, of which it constitutes a technical
revision.
Annexes A and B of this International Standard are for information only.

ISO 14284:1996(E)
INTERNATIONAL STANDARD @ ISO
- Sampling and preparation of samples
Steel and iron
for the determination of Chemical composition
3.2 physical method of analysis: Method for the
1 Scope
determination of Chemical composition in which the
determination of composition is carried out without
This International Standard specifies methods for
submitting the Sample to Chemical reaction, for
sampling and Sample preparation for the determi-
example an Optical emission spectrometric method,
nation of the Chemical composition of pig iron, cast
an X-ray fluorescence spectrometric method.
iron and steel. Methods are specified for use with
both liquid and solid metal.
3.3 thermal method of analysis: Method for the
determination of Chemical composition in which the
Sample is submitted to a process of heating, combus-
tion or fusion.
2 Normative references
The following Standards contain provisions which,
3.4 melt: Liquid metal from which a Sample is re-
through reference in this International Standard. At the
moved.
time of publication, the editions indicated were vaiid.
All Standards are subject to revision, and Parties to
agreements based on this International Standard are
3.5 spoon sampling: Method in which the Sample
encouraged to investigate the possibility of applying
is taken from the melt, or during the pouring of the
the most recent editions of the Standards indicated
melt, using a long-handled spoon, and cast into a
below. Members of IEC and ISO maintain registers of
small mould.
currently valid International Standards.
3.6 spoon Sample: Sample taken from the melt
ISO 377: -11, Steel and steel products - Location of
samples and test pieces for mechanical testing. using a spoon and cast into a small mould.
ISO 9147:1987, Pig-irons - Definition and classifi-
3.7 probe sampling: Method in which the Sample is
ca tion.
taken from the melt using a commercially available
sampling probe inserted into the melt.
3 Definitions
3.8 immersion sampling: Method of probe sam-
pling in which the probe is immersed in the melt
where the Sample chamber in the probe fills by ferro-
For the purposes of this International Standard, the
static pressure or gravity.
following definitions apply.
3.9 suction sampling: Method of probe sampling in
3.1 Chemical method of analysis: Method for the
which the probe is immersed in the melt where the
determination of Chemical composition in which the
Sample chamber in the probe fills by aspiration.
Sample is submitted to Chemical reaction.
1) To be published. (Revision of ISO 377-1 :1989)
ISO 14284:1996(E) @ ISO
3 When the Sample for analysis is in the form of Chips or
3.10 stream sampling: Method of probe sampling
powder, or when a Sample in the form of a solid mass is
in which the probe is inserted into a stream of liquid
analysed by a thermal method, the test Portion is obtained
metal where the Sample chamber in the probe fills by
by weighing. In the case of a physical method of analysis,
the forte of metal flow.
the part actually analysed will constitute only a small mass
of the Sample for analysis. In an Optical emission spectro-
metric method, the mass sf metal consumed in an electri-
3.11 probe Sample: Sample taken from the melt
cal discharge is about 0,5 mg to 1 mg; in an X-ray fluor-
using a commercially available sampling probe.
escence spectrometric method, the characteristic radiation
is produced from a very thin surface layer of the Sample.
3.12 cast product: Item of iron or steel which has
not been subject to deformation, for example, an in-
3.18 grinding: Method of preparing a Sample of
got, a semi-finished product obtained by continuous
metal for a physical method of analysis in which the
casting, a shaped casting.
surface of the Sample for analysis is abraded using an
abrasive wheel.
3.13 wrought product: Item of steel which has
been subject to deformation by rolling, drawing, forg-
3.19 linishing: Method of preparing a Sample of
ing or some other method, for example, a bar, a billet,
metal for a physical method of analysis in which the
a plate, a Strip, a tube, a wire.
surface of the Sample for analysis is abraded using a
flexible rotating disc or continuous belt coated with an
abrasive substance.
3.14 Sample product: Specific item of iron or steel
selected from a supplied quantity for the purpose of
obtaining a Sample.
3.20 milling: Method sf preparing Sample Chips or
the surface of a Sample for a physical method of
analysis in which the surface of the Sample is ma-
3.15 preliminary Sample: Sufficient quantity of
chined using a rotating, multi-edged cutting tool.
metal selected from the Sample product for the pur-
pose of obtaining one or more samples for analysis.
3.21 consignment: Quantity of metal delivered at
one time.
3.16 Sample for analysis: Part of the Sample prod-
uct, or part of the preliminary Sample taken from the
Sample product, or part of the Sample taken from the
3.22 increment: Quantity of metal obtained by
melt, brought to a required condition for Submission to
sampling at one time from a consignment.
analysis.
he Sample for an alysis may compri se the sa mple
roduct itself or the Sample tak en from the melt.
P
4 Requirements for sampling
NOTE 1 The following categories of Sample for analysis
and Sample preparation
are distinguished:
- Sample in the form of a solid mass;
- Sample that has been remelted; 4.1 General
- Sample in the form of Chips obtained by machining;
This clause covers the general requirements for the
- Sample in the form of fragments obtained by commi-
Sample, and for the sampling and Sample preparation
nution;
of iron and steel. Special requirements apply to each
- Sample in the form of powder obtained by comminution.
category of liquid and solid metal and these are con-
sidered in the relevant subclause.
3.17 test Portion: Part of the Sample for analysis, or
part of the Sample taken from the melt, actually sub-
The sequence of sampling and Sample preparation of
mitted to analysis. In certain cases, the test Portion
liquid iron and steel, and cast iron and steel products
may be selected from the Sample product itself.
is shown in figure 1. Special considerations apply to
pig irons (see clause 8).
NOTES
2 The following special types of test portions in the form
4.2 Sample
of a solid mass obtained from a probe Sample are dis-
tinguished:
- test Portion in the shape of a small disc, commonly de- 4.21 Quality
scribed as a slug, obtained by punching;
Sampling practices shall be designed to provide a
- test Portion in the form of a small appendage, com-
monly described as a lug; Sample for analysis that is representative of the mean
Chemical composition of the melt or the Sample
- test Portion in the form of a small-diameter rod, com-
monly described as a pin, obtained by cutting. product.

,
@ ISO ISO 14284:1996(E)
Product batch
Preliminary Sample
Sample for analysis
Sample for analysis
Test Portion
c>
a) Liquid iron and steel b) Cast iron and steel products
Figure 1 - Sequence of sampling and Sample preparation
I ne Sample for analysis shall be sufficiently homo- Particular care shall be taken when selecting and pre-
geneous with respect to Chemical composition such paring the Sample for analysis, where a Sample taken
that inhomogeneity does not appreciably contribute to from a melt is expected to be heterogeneous or con-
the error variability of the method of analysis. How- taminated in any way.
ever, in the case of a Sample taken from a melt, some
variability in analysis, both within and between
A Sample taken from a melt shall be cooled in such a
samples for analysis, may be unavoidable; this varia-
manner that the Chemical composition and metallurgi-
bility will form an inherent part of the repeatability and
cal structure of the Sample is consistent from Sample
reproducibility of the analysis.
to Sample.
be free from surface
The Sample for analysis shal
coatings, and from moisture, dirt or other forms of lt is important to recognize that analysis by some
contamination.
physical methods may be influenced by the metal-
lurgical structure of the Sample, particularly in the
As far as possible, the Sample for analysis should be case of irons with white and grey iron structures, and
free from voids, Cracks and porosity, and from fins, in the case of steels in the as-cast and wrought con-
ditions.
laps or other surface defects.
@ ISO
ISO 14284:1996(E)
4.2.2 Size 4.2.5 Arbitration
The dimensions of a preliminary Sample in the form of In the case of a Sample intended for arbitration, the
a solid mass shall be sufficient to permit additional Sample for analysis shall be prepared jointly by the
samples for analysis to be taken for re-analysis, where supplier and purchaser, or by their representatives. A
necessary using an alternative method of analysis. record shall be kept of the methods used for preparing
the Sample for analysis.
A Sample for analysis, of a sufficient mass to provide
Containers with samples for analysis intended for arbi-
for any re-analysis necessary, shall be prepared. Gen-
tration shall be sealed by both Parties or by their rep-
erally, a mass of 100 g will be sufficient for a Sample
resentatives. Unless agreed to the contrary, these
in the form of Chips or powder.
Containers shall be kept by the representatives of
each Party responsible for the preparation of samples.
The dimensional requirements for a Sample for analy-
sis in the form of a solid mass will depend upon the
method selected for analysis. In the case of Optical
emission and X-ray fluorescence spectrometric
4.3 Selection of a Sample
methods, the shape and size of the Sample will be de-
termined by the dimensions of the Sample chamber.
4.3.1 Sample from a melt
The dimensions for samples for analysis given in this
International Standard should be regarded as indica-
Melts are sampled at various stages in the manufac-
tive only.
turing process for the purposes of monitoring and
controlling the process. Samples tan be taken during
the casting of the melt to verify Chemical composition
in accordance with the specification of the cast prod-
4.2.3 Identification
uct. In the case of liquid metal intended for the pro-
duction of a casting, the Sample for analysis may be
A Sample for analysis shall be assigned a unique
selected from test bars or blocks specially cast from
identification in Order to determine the melt of Sample
the same metal as that of the casting for purposes of
product from which it was taken and, if necessary, the
mechanical testing, in accordance with the product
processing conditions of the melt or the location of
Standard.
the preliminary Sample or the Sample for analysis in
the Sample product.
Sampling practices for melts shall be designed to
provide samples during a particular manufacturing
A Sample for analysis of pig iron shall be assigned a
process in accordance with requirements for Sample
unique identification in Order to determine the con-
quality (see 42.1). The Sample obtained from a melt is
signment or part of a consignment and the increment
usually in the form of a small ingot, a cylindrical or rec-
from which it was taken.
tangular block, a chill-cast disc or a combination of a
disc with one or more attached Pins; in some cases
Labelling or some equivalent method of marking shall
small lugs are attached to a disc Sample.
be used to ensure that the assigned identification
remains associated with the Sample for analysis.
NOTE 4 Sampling probes for use with liquid iron and steel
may be obtained from a number of suppliers; the main fea-
The identification, Status and condition of the Sample
tures of the different types of probe are distinguished in
shall be recorded to ensure that confusion cannot
annexes A and B, which include dimensions for information
arise as to the identity of the item to which analysis
only.
and records refer.
4.3.2 Sample from a product
4.2.4 Conservation
The preliminary Sample or the Sample for analysis tan
be selected from the Sample product at the location
Adequate storage facilities shall be provided to segre-
indicated in the product specification for the selection
gate and protect the Sample for analysis. During and
of material for mechanical testing, when available.
after preparation, the Sample for analysis shall be
stored in such a way as to prevent contamination or
In the case of an iron casting, the Sample for analysis
Chemical Change.
tan be selected from a bar or block cast onto the
casting.
lt is permitted to conserve the preliminary Sample in
the form of a solid mass, and a Sample for analysis
In the case of a forging, the Sample for analysis
may then be prepared when required.
tan be selected from the initial starting material
from which the forging has been made, or from pro-
The Sample for analysis, or the preliminary Sample in
longations of the forging or from additional forgings.
the form of a solid mass, shall be kept for a sufficient
period of time to protect the integrity of the test lab- In the absen ce of requirements given in the product
oratory. standa rd, or of a specification when ordering the
@ ISO ISO 14284:1996(E)
Chips shall be thoroughly mixed before weighing the
product, the Sample for analysis may, following
agreement between the supplier and the purchaser, test Portion. For most purposes, it is satisfactory to
mix the Chips by rolling the Container on a level sur-
be selected from the Sample for mechanical testing
or from the test piece, or directly from the Sample face and/or gently tumbling the Container.
product.
The preliminary Sample or the Sample for analysis tan
4.4.3 Sample for analysis in the form of a powder
be obtained from the Sample product by machining or
or fragments
by using a cutting torch. Special considerations apply
in the case of sampling for the determination of cer-
Where drilling of the Sample to obtain Chips is imprac-
tain elements.
ticable, it shall be tut or broken into pieces. These
pieces shall then be crushed using a percussion mor-
tar or a vibratory grinding mill, also known as a disc
mill or ring mill, to obtain a Sample for analysis in the
4.4 Preparation of a Sample
form of a powder, the whole of which Passes through
a sieve of a specified aperture size.
4.4.1 Preliminary preparation
In some applications for the determination of carbon
If any part of the Sample is liable to be non-
using a thermal method of analysis, the Sample is
representative in Chemical composition, for example
crushed in a percussion mortar to obtain a Sample for
due to Oxidation, it may be agreed, following an inves-
analysis in the form of fragments with a particle size
tigation to establish the nature and extent of any
range of approximately 1 mm to 2 mm.
Change in composition, to remove from the Sample
those Parts that have changed. Following this oper-
Equipment used for comminution shall be constructed
ation, the Sample shall then be protected from any
from material which does not alter the Sample com-
Change in composition.
Position. Suitable tests may be necessary to show
that the use of such equipment does not affect the
If necessary, the surface of the metal shall be laid
composition of the Sample for analysis in any way.
completely bare at the Point of machining, by any
suitable means, to remove any coating that has been
Comminution shall not be used for the preparation of
applied during manufacture. If necessary, the surface
samples of graphite-bearing irons.
of the metal shall be degreased by means of a suit-
able solvent, taken care to ensure that the manner
The sieving Operation shall be performed taking all
of degreasing does not affect the correctness of
precautions necessary to avoid contamination or loss
analysis.
of material. When sieving hard materials, care shall be
taken to avoid damaging the fabric of the sieve.
4.4.2 Sample for analysis in the form of Chips
The Sample for analysis shall be homogenized before
The Sample for analysis shall consist of Chips of a
weighing the test Portion. Powders tan be homogen-
regular size and shape. These may be obtained by
ized by stirring.
methods such as drilling, milling, turning or punching.
The Chips shall not be taken from a part of the Sample
CAUTION - Finely-divided metals of particle size
that has been affected by the heat of a cutting torch.
less than approximately 150 Pm tan present a fire
risk. Ensure that there is adequate Ventilation
The tools, machines and Containers used during
during comminution.
preparation of the Sample shall be cleaned beforehand
to prevent any contamination of the Sample for analy-
4.4.4 Sample for analysis in the form of a solid
mass
Machining shall be carried out in such a way that the
Chips are not subject to overheating, as indicated by a
4.4.4.1 Selection of the Sample for analysis
Change in the colour (blueing or blackening) of the
Chips. Unavoidable coloration of Chips obtained from
The Sample for analysis shall be obtained by cutting,
some types of alloy steels, for example manganese
from the Sample product or preliminary Sample, a
and austenitic steels, tan be minimized by selection of
piece of size and shape suitable for the method of
appropriate tools and cutting Speeds.
analysis. Samples shall be tut by sawing, abrasive
cutting, shearing or punching.
Heat treatment may be required to soften the Sample
for machining.
In the absence of any indication in the product stan-
dard, analysis by a physical method shall be carried
The use of coolants during machining is only permit-
out on that part of the Sample corresponding to a
ted in exceptional cases; after which the Chips shall be
transverse section of the product, provided that the
cleaned by means of a suitable solvent which does
material has sufficient thickness.
not leave any deposit.
0 ISO
ISO 14284:1996(E)
4.4.4.2 Surface preparation of the Sample method selected for surface preparation produces
for analysis a grade of surface finish that is reproducible from
Sample to Sample. In addition, there should be no
smearing of the surface.
The Sample for analysis shall be prepared to expose a
surface suitable for the method of analysis. Prep-
aration of a surface for analysis shall not be carried out
The effect of abrasive materials depends on the ana-
on any part of a Sample that has been affected by
lytical method. When using Optical emission spectro-
the heat of a cutting torch. The equipment used for
metric methods, the action of presparking will nor-
Sample preparation shall be designed to minimize
mally clean the surface of the Sample for analysis by
overheating the Sample and, where appropriate, shall
volatilizing any grinding contaminants. However, par-
incorporate Systems of cooling.
ticular care is required to avoid surface contamination
when using a new abrasive disc
Four main types of equipment used for surface prep-
aration may be distinguished.
When using X-ray fluorescence spectrometric methods,
all the phases of surface preparation shall be exam-
a) A milling machine capable of removing a pre-
ined for potential surface contamination effects.
selected depth of metal in a reproducible manner,
for use with samples that are within a hardness
The Sample for analysis shall be examined visually
range suitable for milling. The equipment should
after preparation to establish that the surface is free
be able to be used, if required, with a Sample
from particulate matter and that there are no defects;
taken from a melt where the Sample is still hot.
the Sample shall be resurfaced or discarded if defects
are present. The Sample for analysis shall be dry and
A grinding machine with a fixed, rotating or oscil-
b)
care shall be taken to protect the prepared surface
lating head capable of removing a preselected
from contamination.
depth of metal in a reproducible manner.
c) A flat-bed linishing machine with abrasive grinding
discs, or a machine with continuous abrasive-
Preparation of a Sample for analysis
4.4.5
belts, able to be used to prepare the surface of
by remelting
the Sample for analysis to varying grades of finish.
A Sample in the form of small pieces or Chips, or a
d) A machine for blasting with Sand, grit, or metal
part of the Sample product itself, tan be remelted in
shot, able to be used in special applications to
an atmosphere of argon using commercially available
clean the surface of the Sample for analysis or the
melting equipment. The Sample is converted into a
test Portion.
disc, 40 mm to 30 mm in diameter and 6 mm thick,
which is suitable for analysis by a physical method.
the surface of the Sample for
After preparation,
Some types of remelting equipment incorporate facili-
analysis shall be flat and free from defects which
ties for the centrifugal casting of the disc.
affect the correctness of analysis.
Partial losses of some elements tan be experienced
Cutting and surface preparation tan be performed
during the remelting process. lt is essential to ensure
either manually or automatically. In the case of
that any selective volatilization or Segregation of el-
samples taken from melts, commercially available
ements, or any other Change in composition, which
Systems, which perform each Stage of preparation
occurs is quantitatively known and does not signifi-
automatically, may be used. Systems for the auto-
cantly influence the analysis results. Suitable tests
matic preparation of surfaces of dual-thickness probe
shall be carried out to show that any Change in com-
samples [see A.Z.3 c) in annex Al, and for the punch-
Position is both small in magnitude and reproducible.
ing of slugs forming test portions, may incorporate
facilities for the sand-blasting of the Sample and for
The equipment used and the method adopted for
heat treatment to soften the Sample before punching.
remelting shall be designed to prevent or minimize a
Change in composition and to ensure that any Change
The abrasive substances used in the final Stage of
is reproducible. A deoxidant, for example 0,l % (mlpn)
preparing the Sample for analysis shall be selected so
zirconium, should be used during remelting. The
as to avoid contaminating the surface with elements
method used for calibration of the analytical measure-
that are to be determined by the analysis method. The
ment shall take account of any Change that does
grit size of the abrasive shall be in accordance with
occur.
the grade of surface finish required for the analysis
method.
Not all ferrous metals tan be remelted in this manner.
This method shall not be used for Sample preparation
In the case of Optical emission spectrometric methods,
for the determination of an element which is subject
an abrasive with a grade of 60 grit to 120 grit is nor-
to a significant and non-reproducible Change in com-
mally suitable. In the case of X-ray fluorescence spec-
Position, when remelted.
trometric methods, it is essential to ensure that the
@ ISO ISO 14284:1996(E)
5.2 Spoon sampling
4.5 Safety precautions
5.2.1 Methods
4.5.1 Personal protection
For sampling from a melt, immerse a preheated steel
Personal protective equipment shall be provided
spoon into the melt and fill with liquid iron. Withdraw
to minimize the risk of injury during sampling and
the spoon and remove any slag by skimming the sur-
Sample preparation methods. Provisions shall in-
face of the liquid iron in the spoon.
clude protective clothing, hand protection and
face visors resistant to splashes, for use during
For sampling from a stream, introduce a preheated
the sampling sf liquid metal. Provisions shall also
steel spoon into the stream from the ladle and fill it
include protective clothing, hand, eye and hearing
with liquid iron.
protection, for use during the sampling and
Sample preparation of solid metal; and respiratory
Pour the liquid iron from the spoon without delay into
protection for use where necessary.
a metal mould to chill the iron as rapidly as possible.
Remove the Sample from the mould and break off any
riser.
4.5.2 Machinery
lt is essential that the liquid iron should be poured into
a mould that is cold to ensure adequate chilling; if
The use of machinery for sampling and Sample
necessary, the mould should be air-cooled before use.
preparation shall be in accordance with appro-
The mould shall be free from moisture.
priate national Standards. Grinding operations
used for surface preparation may be covered by
A disc-shaped Sample, commonly described as a coin
national legislation.
Sample, tan be obtained using a two-piece steel
mould; the Sample in typically 35 mm to 40 mm in di-
ameter with a thickness varying from 6 mm to
12 mm. The mould is constructed in two pieces which
4.5.3 Hazardous substances
are clamped together while in use: one piece is a flat
chill plate, the other is a block with the mould cavity.
appropriate national
Reference shall be made to
The edge of the mould cavity may be tapered, for
the use of solvents
regulations with regard to
example, from 38 mm to 32 mm, to facilitate removal
sf samples and test
for the cleaning and drying
of the Sample from the mould. A coin Sample is verti-
portions.
cally or horizontally cast in the mould.
A coin Sample with one or more attached pins tan be
obtained using a combination-type mould. The pins
are broken off from the disc and used, if required,
m =
5 Liquid iron for steelmawng ana as test portions for analysis by a thermal method.
(A combination-type mould for use with liquid iron
pig-iron production
intended for the production of cast iron is shown in
figure 2.)
5.1 General
A thin slab-shaped Sample with a rounded end tan be
The following methods are applicable to the sampling obtained using a cast iron or steel Split-mould; the di-
mensions of the Sample are typically 70 mm x 35 mm
of liquid blast-furnace iron intended for steelmaking,
with a thickness of 4 mm. The two halves of the
and commonly described as hot metal, or for the
mould are bevelled at the top to give a feeder head
casting of pig-iron. The liquid iron is normally sampled
and are clamped together while in use. This type of
from the blast furnace runner while the melt is poured
mould may be preferred for use with liquid iron con-
into torpedo ladles, or from transfer vessels, or during
taining high percentages of carbon.
secondary treatment processes in the ladle, or during
the casting of the melt into pig-iron.
The Chemical composition of iron may fluctuate during
5.2.2 Maintenance of equipment
run-out from the blast furnace. Two or more samples
should be taken from the melt at timed intervals and
lt is essential to keep sampling spoons and metal
an average analysis determined.
moulds clean and dry. After use, remove any slag and
skull and clean the surfaces of the mould with a wire
When physical methods are used for analysis, the brush.
method of sampling should be designed to chill the
liquid metal in a manner which ensures that the metal-
Moulds should be remachined if the internal surfaces
lurgical structure of the Sample is suitable for the re-
become worn. This avoids the need for additional ma-
quirements of the analysis method selected.
chining of the Sample during surface preparation.

ISO 14284:1996(E) @ ISO
5.4.3 Sample for analysis by a thermal method
5.3 Probe sampling
Break the pin of a disc-shaped Sample into pieces of a
5.3.1 General
suitable mass for use as test portions, or use the lugs
of a probe Sample. Analyse a representative number
The different types of probes used for sampling blast
of test portions to obtain an average value.
furnace iron are described in annex A. Probes should
be designed to provide a disc-shaped Sample with a
Alternatively, crush the pin or Iugs in a percussion
white iron structure which is sufficiently deep for the
mortar to obtain a sufficient mass of Sample for
requirements of the physical method selected for
analysis of particle size approximately 1 mm to 2 mm.
analysis.
Avoid the production of fine material during crushing.
In the case of a slab-shaped Sample, break the Sample
Probe sampling is influenced by such factors as the
into small pieces and crush the pieces in a similar
angle and depth of immersion of the Sampler in the
manner.
melt, and immersion times tan vary depending on the
temperature of the liquid iron. These factors should be
determined for the particular ironmaking practice and
5.4.4 Sample for analysis by a physical method
thereafter strictly controlled to maintain the Standard
of quality of the Sample for analysis.
In the case of a disc-shaped Sample, remove any lugs
or Pins, as necessary, and then grind the surface of
the Sample to expose a white iron structure which is
representative of the Sample. The amount of material
5.3.2 Methods
to be removed in this way shall be determined for the
Chemical composition of the particular iron and the
For sampling from a melt, immerse a suitable immer-
conditions of sampling; the thickness of the layer to
sion probe Sampler into the melt at an angle as near
be removed normally lies between 0,5 mm and 1 mm
as possible to the vertical plane.
(see A.6).
When sampling from the runner of a blast furnace,
ln the case of a slab-shaped Sample, break the slab
select the Position of immersion to give a sufficient
into two pieces to obtain a Sample of suitable size for
depth of liquid metal for the use of a probe Sampler.
analysis.
A depth of approximately 200 mm is adequate for
most types of sampling probe.
Prepare the surface of the Sample by grinding and lin-
ishing. Grinding shall be carried out wet to avoid over-
For sampling from a stream of liquid iron, introduce a
heating the Sample but the final surface preparation
suitable suction probe Sampler into the metal flow
shall be dry linishing. Alternatively, cool the Sample
from a ladle, at an angle of approximately 45” to the
after grinding by immersion in water and then finish
vertical plane, at a Position as near as possible to the
by dry linishing.
nozzle of the vessel.
Particular care is required when preparing the surface
Withdraw the probe Sampler from the melt after a
of thin samples. A chuck shall be specially designed to
predetermined interval of time, break it apart and
hold the Sample securely grinding and linishing oper-
allow the Sample to cool in air.
ations.
5.4 Preparation of a Sample for analysis
6 Liquid iron for cast iron production
5.4.1 Preliminary preparation
6.1 General
Remove any surface Oxidation from a Sample taken
from the melt, that may contaminate the Sample for
The following methods are applicable to the sampling
analysis during subsequent preparation.
of liquid iron from cupola furnaces and electric fur-
naces, from holding furnaces in duplex processes, and
from ladles and treatment vessels.
5.4.2 Sample for analysis by a Chemical method
Liquid iron intended for the production of iron castings
Break the Sample into small pieces and crush pieces may be subject to inhomogeneity, and particular care
using a percussion mortar or a vibratory grinding mill is requ
...