This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: E1806 − 23

Standard Practice for

Sampling Steel and Iron for Determination of Chemical
Composition1
This standard is issued under the fixed designation E1806; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope
Sections
1.1 This practice covers the sampling of all grades of steel, Steel Products 12
both cast and wrought, and all types (grades) of cast irons and General 12.1
blast furnace iron for chemical and spectrochemical determi- Selection of a Laboratory Sample or a Sample for 12.2
Analysis from a Cast Product
nation of composition. This practice is similar to ISO 14284. Selection of a Laboratory Sample or a Sample for 12.3
Analysis from a Wrought Product
1.2 This practice is divided into the following sections. Preparation of a Sample for Analysis 12.4
Sections Sampling of Leaded Steel 12.5
Requirements for Sampling and Sample Preparation 6 Sampling and Sample Preparation for the Determination 12.6
General 6.1 of Oxygen
Sample 6.2
Selection of a Sample 6.3 Sampling and Sample Preparation for the Determination 12.7
Preparation of a Sample 6.4 of Hydrogen

Liquid Iron for Steelmaking and Pig Iron Production 7 Keywords 13

General 7.1
Spoon Sampling 7.2 Annexes
Probe Sampling 7.3 Sampling Probes for Use with Liquid Iron and Steel Annex A1
Preparation of a Sample for Analysis 7.4 Sampling Probes for Use with Liquid Steel for the Annex A2
Determination of Hydrogen
Liquid Iron for Cast Iron Production 8
General 8.1
1.3 The values stated in SI units are regarded as standard.
Spoon Sampling 8.2 No other units of measurement are included in this standard.
Probe Sampling 8.3
Preparation of a Sample for Analysis 8.4
1.4 This standard does not purport to address all of the
Sampling and Sample Preparation for the Determination of 8.5 safety concerns, if any, associated with its use. It is the
Oxygen and Hydrogen responsibility of the user of this standard to establish appro-
Liquid Steel for Steel Production 9
priate safety, health, and environmental practices and deter-
General 9.1 mine the applicability of regulatory limitations prior to use.
Probe Sampling 9.2 For specific statements, see 6.4.3.5, 9.4.4.3, 12.5.1, and Section
Spoon Sampling 9.3
Preparation of a Sample for Analysis 9.4
5.
Sampling and Sample Preparation for the Determination 9.5 1.5 This international standard was developed in accor-
of Oxygen dance with internationally recognized principles on standard-
Sampling and Sample Preparation for the Determination 9.6
of Hydrogen ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
Pig Irons 10 mendations issued by the World Trade Organization Technical
General 10.1
Increment Sampling 10.2 Barriers to Trade (TBT) Committee.
Preparation of a Sample for Analysis 10.3
2. Referenced Documents
Cast Iron Products 11
General 11.1 2.1 ASTM Standards:2
Sampling and Sample Preparation 11.2 A48/A48M Specification for Gray Iron Castings
A751 Test Methods and Practices for Chemical Analysis of
Steel Products
1
This practice is under the jurisdiction of ASTM Committee E01 on Analytical
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
2
Subcommittee E01.01 on Iron, Steel, and Ferroalloys. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2023. Published July 2023. Originally approved contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
in 1996. Last previous edition approved in 2018 as E1806 – 18. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
E1806-23. the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 E1806 − 23
E135 Terminology Relating to Analytical Chemistry for 3.2.14 test portion, n—part of the sample for analysis, or
Metals, Ores, and Related Materials part of the sample taken from the melt, actually analyzed.
E415 Test Method for Analysis of Carbon and Low-Alloy 3.2.14.1 Discussion—Sometimes, the test portion may be
Steel by Spark Atomic Emission Spectrometry selected from the sample product itself.
E1306 Practice for Preparation of Metal and Alloy Samples 3.2.15 thermal method of analysis, n—method for the de-
by Electric Arc Melting for Spectrochemical Analysis termination of chemical composition in which the sample is
2.2 ISO Standards: submitted to a process of heating, combustion, or fusion.
ISO 9147 Pig irons–Definition and classification3 3.2.16 wrought product, n—item of steel which has been
ISO 14284 Steel and iron—Sampling and preparation of subject to deformation by rolling, drawing, forging, or some
samples for the determination of chemical composition3 other method, for example, a bar, billet, plate, strip, tube, or
wire.
3. Terminology
3.1 Definitions—For definitions of terms in this practice, 4. Significance and Use
refer to Terminology E135. 4.1 This practice covers all aspects of sampling and prepar-
3.2 Definitions of Terms Specific to This Standard: ing steel and iron for chemical analysis as defined in Test
3.2.1 cast product, n—item of iron or steel which has not Methods, Practices, and Definitions A751 and Specification
been subject to deformation, for example, an ingot, a semi A48/A48M. Such subjects as sampling location and the sam-
finished product obtained by continuous casting, or a shaped pling of lots are defined.
casting. 4.2 This practice includes most requirements for sampling
3.2.2 consignment, n—quantity of metal delivered at one steel and iron for analysis. Standard test methods that reference
time. this practice need contain only special modifications and
3.2.3 grinding, n—method of preparing a sample of metal exceptions.
for a spectrochemical method of analysis in which the surface 4.3 All who use these procedures should be trained samplers
of the sample is abraded using an abrasive wheel. capable of performing common sampling operations skillfully
3.2.4 linishing, n—method of preparing a sample of metal and safely. Only proper sampling equipment should be used.
for a spectrochemical method of analysis in which the surface
of the sample is abraded using a rotating disk or belt coated 5. Hazards and Safety Precautions
with an abrasive substance. 5.1 Provide personal protective equipment to minimize the
3.2.5 melt, n—liquid metal from which a sample is re- risk of injury during sampling and sample preparation meth-
moved. ods. Provisions shall include protective clothing, hand
3.2.6 sample, probe, n—sample taken from the melt using a protection, and face visors resistant to splashes of liquid metal
sampling probe. for use during the sampling of liquid metal; protective clothing
and hand, eye, and hearing protection for use during the
3.2.7 sample, product, n—specific item of iron or steel sampling and sample preparation of solid metal; and respira-
selected from a supplied quantity for the purpose of obtaining tory protection for use where necessary.
a sample.
5.2 The use of machinery for sampling and sample prepa-
3.2.8 sample, spoon, n—sample taken from the melt using a
ration shall be in accordance with appropriate national stan-
spoon and cast into a small mold.
dards. Grinding operations used for surface preparation may be
3.2.9 sampling, immersion, n—method of probe sampling in covered by national legislation.
which the probe is immersed in the melt and the sample
5.3 Refer to appropriate national regulations regarding the
chamber in the probe fills by ferrostatic pressure or gravity.
use of solvents for cleaning and drying of samples and test
3.2.10 sampling, probe, n—method in which the sample is portions.
taken using a sampling probe inserted into the melt.
3.2.11 sampling, spoon, n—method in which the sample is 6. Requirements for Sampling and Sample Preparation
taken from the melt, or during the pouring of the melt, using a 6.1 General:
long-handled spoon and cast into a small mold. 6.1.1 This section describes the general requirements for the
3.2.12 sampling, stream, n—method of probe sampling in sample and for the sampling and sample preparation of iron
which the probe is inserted into a stream of liquid metal and the and steel. Special requirements apply to each category of liquid
sample chamber in the probe fills by force of metal flow. and solid metal, and these requirements are described in the
3.2.13 sampling, suction, n—method of probe sampling in relevant section.
which the probe is inserted into the melt and the sample 6.1.2 The sequence of sampling and sample preparation of
chamber in the probe fills by aspiration. liquid iron and steel and cast iron and steel products is shown
in Fig. 1. Special considerations apply to pig irons (see Section
10).
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 6.2 Sample:
4th Floor, New York, NY 10036, http://www.ansi.org. 6.2.1 Quality:

2
 E1806 − 23

FIG. 1 Sequence of Sampling and Sample Preparation of (a) Liquid Iron and Steel and (b) Cast Iron and Steel Products

6.2.1.1 Sampling practices shall be designed to provide an 6.2.1.6 A sample taken from a melt shall be cooled in such
analytical sample that is representative of the mean chemical a manner that the chemical composition and metallurgical
composition of the melt or of the sample product. structure of the sample is consistent from sample to sample.
6.2.1.2 Ensure that the sample is sufficiently homogeneous 6.2.1.7 It is important to recognize that analysis by some
regarding chemical composition so that inhomogeneity does spectrochemical methods may be influenced by the metallur-
not appreciably contribute to the error variability of the method gical structure of the sample, particularly for irons with white
of analysis. For a sample taken from a melt, however, some and grey iron structures, and steels in the as-cast and wrought
variability in analysis, both within and between samples, may conditions.
be unavoidable. This variability will form an inherent part of 6.2.2 Size:
the repeatability and reproducibility of the analysis. 6.2.2.1 Ensure that the dimensions of a laboratory sample in
6.2.1.3 Ensure that the sample is free from surface coatings the form of a solid mass are sufficient to permit additional
and from moisture, dirt, or other forms of contamination. samples to be taken for reanalysis when necessary using an
6.2.1.4 The sample should be free from voids, cracks, and alternative method of analysis.
porosity and from fins, laps, or other surface defects. 6.2.2.2 A sample shall be prepared consisting of a sufficient
6.2.1.5 Take particular care when selecting and preparing mass to provide for any reanalysis necessary. Generally, a mass
the sample if a sample taken from a melt is expected to be of 100 g will be sufficient for a sample in the form of chips or
heterogeneous or contaminated in any way. powder.

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 E1806 − 23
6.2.2.3 The dimensional requirements for a sample in the include dimensions for information only.
form of a solid mass will depend upon the method selected for 6.3.2 Sample from a Product:
analysis. For spark atomic emission and X-ray fluorescence 6.3.2.1 The laboratory sample can be selected from the
spectrometric methods, the shape and size of the sample will be sample product at the location indicated in the product speci-
determined by the dimensions of the sample chamber. The fication for the selection of material for mechanical testing
dimensions for samples given in this practice are for guidance when available.
only. Refer to Test Method E415 for sample size requirements 6.3.2.2 For an iron casting, the sample can be selected from
for spark atomic emission spectrometry. a bar or block cast-on to the casting.
6.2.3 Identification: 6.3.2.3 For a forging, the sample can be selected from the
6.2.3.1 Assign the sample a unique identification to deter- initial starting material from which the forging has been made
mine the melt or sample product from which it was taken, and or from prolongations of the forging or from additional
if necessary, the process conditions of the melt or the location forgings.
of the laboratory sample in the sample product. For pig iron, 6.3.2.4 In the absence of requirements given in the product
this shall identify the consignment or part of a consignment and standard or of a specification when ordering the product, the
the increment from which it was taken. sample may, following agreement between the supplier and the
6.2.3.2 Use labeling or some equivalent method of marking purchaser, be selected from the sample for mechanical testing
to ensure that the assigned identification remains associated or from the test piece, or directly from the sample product.
with the sample. 6.3.2.5 The laboratory sample can be obtained from the
6.2.3.3 Record the identification of the sample to ensure that sample product by machining or by using a cutting torch.
confusion is prevented regarding the identity of the item to Special considerations apply to sampling for the determination
which the analysis and records refer. of certain elements.
6.2.4 Conservation:
6.4 Preparation of a Sample:
6.2.4.1 Provide adequate storage facilities to segregate and
6.4.1 Preliminary Preparation:
protect the sample. During and after preparation, store the
6.4.1.1 If any part of the sample is potentially nonrepresen-
sample in a manner which prevents contamination or chemical
tative in chemical composition, remove those parts that have
change.
changed. Following this operation, the sample shall be pro-
6.2.4.2 Keep the sample, or the laboratory sample in a solid
tected from any change in composition.
mass form, for a sufficient period of time to permit retesting if
6.4.1.2 Remove any coating that has been applied during
necessary.
manufacturing. If necessary, degrease the surface of the metal
6.2.5 Arbitration:
with a suitable solvent, taking care to ensure that the manner of
6.2.5.1 Samples intended for arbitration shall be prepared
degreasing does not affect the accuracy of analysis.
jointly by the supplier and purchaser or by their representa-
6.4.2 Sample in the Form of Chips:
tives. Keep a record of the methods used for preparing samples.
6.4.2.1 Obtain the sample by drilling, milling or turning to
6.2.5.2 Both parties or their representatives shall seal con-
produce chips of a consistent size and shape. Do not machine
tainers with the samples intended for arbitration. Unless agreed
on a part of the sample that has been affected by the heat of a
to the contrary, the representatives of each party responsible for
cutting torch.
the preparation of samples will keep these containers.
6.4.2.2 Before preparation, clean the tools, machines, and
6.3 Selection of a Sample: containers to be used during preparation to prevent any
6.3.1 Sample from a Melt: contamination of the sample.
6.3.1.1 Melts are sampled at various stages in the manufac- 6.4.2.3 Machine in such a way that the chips are not subject
turing process for the purposes of monitoring and controlling to overheating as indicated by a change in the color (blueing or
the process. Samples can be taken during the casting of the blackening). Unavoidable coloration of chips obtained from
melt to verify chemical composition in accordance with the some types of alloy steels, for example, manganese and
specification of the cast product. For liquid metal intended for austenitic steels, can be minimized by selection of appropriate
the production of a casting, the analytical sample may be tools and cutting speeds.
selected from test bars or blocks specially cast from the same 6.4.2.4 Heat treatment may be required to soften the sample
metal as that of the casting for purposes of mechanical testing for machining.
in accordance with the product standard. 6.4.2.5 The use of coolants during machining is only per-
6.3.1.2 Sampling practices shall be designed for melts to mitted in exceptional cases, after which the chips shall be
provide samples during a particular manufacturing process in cleaned by means of a suitable solvent that does not leave any
accordance with requirements for sample quality (see 6.2.1). residue.
The sample obtained from a melt is usually a small ingot, a 6.4.2.6 Mix the chips thoroughly before weighing the test
cylindrical or rectangular block, or a chill-cast disk or a portion. For most purposes, it is satisfactory to mix the chips by
combination of a disk with one or more attached pins. rolling the container on a level surface, gently tumbling the
Sometimes small lugs are attached to a disk sample. chips.
NOTE 1—Sampling probes for use with liquid iron and steel may be 6.4.3 Sample in the Form of a Powder or Fragments:
obtained from a number of suppliers. The main features of the different 6.4.3.1 If drilling the sample to obtain chips is
types of probe are distinguished in Annex A1 and Annex A2, which impracticable, cut or break the sample into pieces. Crush the

4
 E1806 − 23
pieces using a percussion mortar or a vibratory grinding mill, samples (see A2.3) and for the punching of slugs as test
also known as a disk mill or ring mill, to obtain a sample in the portions may incorporate operations for the sandblasting of the
form of a powder the whole of which passes through a sieve of sample and for heat treatment to soften the sample before
a specified aperture size. punching.
6.4.3.2 In some applications the sample is crushed in a 6.4.5.7 Select the abrasive substances used in the final stage
percussion mortar to obtain a sample in the form of fragments of preparing the sample that do not contaminate the surface
suitable for use with the selected method of analysis. with elements that are to be determined by the analysis method.
6.4.3.3 Equipment used for pulverization shall be con- Ensure that the grit size of the abrasive is in accordance with
structed from material that does not alter the sample compo- the grade of surface finish required for the analysis method.
sition. Tests may be necessary to show that such equipment 6.4.5.8 For spark atomic emission spectrometric methods,
does not affect the composition of the sample. an abrasive with a size of 60 grit to 120 grit normally is
6.4.3.4 Sieve the sample taking precautions to avoid con- suitable. For X-ray fluorescence spectrometric methods, it is
tamination or loss of material. Take care when sieving hard essential to ensure that the method selected for surface prepa-
materials to avoid damaging the fabric of the sieve. ration produces a grade of surface finish that is sufficiently
6.4.3.5 Homogenize the sample before weighing the test smooth and reproducible from sample to sample. Also, there
portion. Powders can be homogenized by stirring. (Warning— should be no smearing of the surface.
Finely divided metals of particle size less than approximately 6.4.5.9 The effect of abrasive materials depends on the
150 µm can present a fire risk. Ensure adequate ventilation analytical method. When using spark atomic emission spectro-
during pulverization.) metric methods, the action of pre-sparking normally will clean
6.4.4 Sample in the Form of a Solid Mass: the surface of the sample for analysis by volatilizing any
6.4.4.1 Obtain the sample by cutting from the sample grinding contaminants. Particular care is required, however, to
product or laboratory sample a piece of suitable size and shape avoid surface contamination when using new abrasive media.
for the method of analysis. Cut samples by sawing, abrasive
6.4.5.10 When using X-ray fluorescence spectrometric
cutting, shearing, or punching.
methods, examine all phases of surface preparation for poten-
6.4.4.2 In the absence of any indication in the product
tial surface contamination effects.
standard, perform a spectrochemical analysis on that part of the
sample corresponding to a transverse section of the product, 6.4.5.11 Examine the sample visually after preparation to
provided that the material has sufficient thickness. establish that the surface is dry and free from particulate matter
and that there are no defects. Resurface or discard the sample
6.4.4.3 Prepare the sample to expose a surface suitable for
if defects are present. Protect the prepared surface from
the analytical method. Do not prepare a surface for analysis on
contamination.
part of a sample that has been affected by the heat of a cutting
torch. The equipment used for sample preparation shall be 6.4.6 Preparation of a Sample for Analysis by Melting:
designed to minimize overheating the sample, and, where 6.4.6.1 A sample in the form of small pieces or chips, or a
appropriate, shall incorporate systems of cooling. part of the sample product itself, can be melted in an atmo-
6.4.5 Main Types of Equipment Used for Surface Prepara- sphere of argon using commercially available melting equip-
tion: ment of the type described in Practice E1306. The sample is
6.4.5.1 A milling machine capable of removing a prese- converted into a disk, 40-mm to 30-mm diameter by 6 mm
lected depth of metal in a reproducible manner, for use with thick, which is suitable for analysis by a spectrochemical
samples that are within a hardness range suitable for milling. method. Some types of melting equipment incorporate opera-
The equipment should be capable of use, if required, with a tions for the centrifugal casting of the disk sample.
sample taken from a melt while the sample is still hot. 6.4.6.2 Partial losses of some elements can be experienced
6.4.5.2 A grinding machine with a fixed, rotating, or oscil- during the melting process. It is essential to ensure that any
lating head capable of removing a preselected depth of metal in selective volatilization or segregation of elements, or any other
a reproducible manner. change in composition, which occur are known quantitatively
6.4.5.3 A flatbed linishing machine with abrasive grinding and do not significantly influence the analysis results. Conduct
disks, or machines with continuous abrasive belts, capable of suitable tests to show that any change in composition is both
preparing the surface of the sample to varying grades of finish. small in magnitude and reproducible.
6.4.5.4 A machine for blasting with sand or grit, or metal 6.4.6.3 The equipment used and the method adopted for
shot, capable of cleaning the surface of the sample or the test melting shall be designed to prevent or minimize change in
portion when required. composition and to ensure that any change is reproducible. A
6.4.5.5 Ensure that the surface of the sample after prepara- deoxidant, for example 0.1 % (m ⁄m) zirconium, should be
tion is flat and free from defects that could affect accuracy of used during melting. Consider any change that does occur
analysis. when using the method for calibration of analytical measure-
6.4.5.6 Cutting and surface preparation can be performed ment.
either manually or automatically. For samples taken from 6.4.6.4 Not all ferrous metals can be melted in this manner.
melts, commercially available systems may be used that Do not use melting as a method of sample preparation for the
perform each stage of preparation automatically. Systems for determination of an element that is subject to a significant and
the automatic surface preparation of dualthickness probe nonreproducible change in composition.

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 E1806 − 23
7. Liquid Iron for Steelmaking and Pig Iron Production
7.1 General:
7.1.1 The following methods are applicable for sampling
liquid blast-furnace iron intended for steelmaking, and com-
monly described as hot metal, or for the casting of pig iron. The
liquid iron is normally sampled from the blast furnace runner
during the pouring of the melt into torpedo ladles, or from
transfer vessels or during secondary treatment processes in the
ladle, or during the casting of the melt into pig iron.
7.1.2 The chemical composition of iron may fluctuate dur-
ing run-out from the blast furnace. Two or more samples
should be taken from the melt at timed intervals and an average
analysis determined.
7.1.3 When spectrochemical methods are used for analysis,
the method of sampling should be designed to chill the liquid
metal in a manner that ensures that the metallurgical structure
of the sample is suitable for the requirements of the analysis
method selected.
7.2 Spoon Sampling: All dimensions are in millimetres.
7.2.1 Hold Types: The flat chill plate (not shown) has similar overall dimensions.
FIG. 2 Combination-Type Vertical Mold Used for Sampling Liquid
7.2.1.1 A disk-shaped sample, commonly described as a Iron Intended for Cast Iron Production
coin sample, can be obtained using a two-piece steel mold. The
dimensions of the sample are typically 35 mm to 40 mm in
diameter with thickness varying from 6 mm to 12 mm. The 7.2.3.1 It is essential to maintain sampling spoons and
mold is constructed in two pieces that are clamped together in molds in a clean and dry condition. After use, remove any slag
use: one piece is a flat chill plate and the other is a block with and skull and brush the faces of the mold with a wire brush.
the mold cavity. The edge of the mold cavity may be tapered, 7.2.3.2 Molds should be re-machined if the internal surfaces
for example, from 38 mm to 32 mm, to facilitate removal of the become worn. This avoids the need for additional machining of
sample from the mold. the sample during surface preparation.
7.2.1.2 A coin sample with one or more attached pins can be 7.3 Probe Sampling:
obtained using a combination-type mold. The pins are broken 7.3.1 General:
off from the disk and used, if required, as test portions for 7.3.1.1 The different types of probes used for sampling blast
analysis by a thermal method. A combination-type mold for use furnace iron are described in Annex A1. Probes are designed to
with liquid iron intended for the production of cast iron is provide a disk-shaped sample with a depth of white iron
shown in Fig. 2. structure that is sufficient for the requirements of the spectro-
7.2.1.3 A thin slab-shaped sample with a rounded end can chemical method selected for analysis.
be obtained using a cast iron or steel split-mold. The dimen- 7.3.1.2 Probe sampling is influenced by such factors as the
sions of the sample are typically 70 mm by 35 mm with a angle and depth of immersion of the sampler in the melt, and
thickness of 4 mm. The two halves of the mold are bevelled at immersion times can vary depending on the temperature of the
the top to give a feeder head and are clamped together in use. liquid iron. These factors should be determined for the particu-
This type of mold may be preferred for use with liquid iron lar iron-making practice, and thereafter, strictly controlled to
containing high amounts of carbon. maintain the standard of quality of the sample.
7.2.2 Procedures: 7.3.2 Procedures:
7.2.2.1 For sampling from a melt, immerse a preheated steel 7.3.2.1 For sampling from a melt, immerse a suitable
spoon into the melt and fill with liquid iron. Withdraw the immersion probe sampler into the melt at an angle as near as
spoon and remove any slag by skimming the surface of the possible to the vertical plane.
liquid iron. 7.3.2.2 When sampling from the runner of a blast furnace,
7.2.2.2 For sampling from a stream, introduce a pre-heated select the position of immersion to give sufficient depth of
steel spoon into the stream from the ladle and fill with liquid liquid metal for the use of a probe sampler. A depth of
iron. approximately 200 mm is adequate for most types of sampling
7.2.2.3 Pour the liquid iron from the spoon without delay probe.
into a metal mold to chill the iron as rapidly as possible. 7.3.2.3 For sampling from a stream of liquid iron, introduce
Remove the sample from the mold and break off any riser. a suitable suction probe sampler into the metal flow from a
7.2.2.4 It is essential that the liquid iron be poured into a ladle, at an angle of approximately 45° to the vertical plane, at
mold that is cold to ensure adequate chilling. If necessary, the a position as near as possible to the nozzle of the vessel.
mold should be air-cooled before use. The mold should be free 7.3.2.4 Withdraw the probe sampler from the melt after a
from moisture. predetermined interval of time, break it apart, and allow the
7.2.3 Maintenance of Equipment: sample to cool in air.

6
 E1806 − 23
7.4 Preparation of a Sample for Analysis: average analysis determined. In continuous processes, samples
7.4.1 Preliminary Preparation—Remove any surface oxida- should be taken at regular intervals of time.
tion from a sample taken from the melt that may contaminate 8.1.4 Methods of sampling normally are designed to chill
the sample during subsequent preparation. the liquid metal of a sample cast from a spoon, as rapidly as
7.4.2 Sample for Analysis by a Chemical Method: possible, to produce a metallurgical structure of white iron free
7.4.2.1 Break the sample into small pieces and crush pieces from graphite. A white iron structure obtained by chill-casting
using a percussion mortar or a vibratory grinding mill to obtain is required generally for analysis by spectrochemical methods.
a sufficient mass of sample of particle size less than 150 µm. 8.1.5 Non-chilled samples also may be used. These samples
7.4.2.2 Alternatively, obtain chips by drilling the sample at can be cast from a spoon, or selected from a test bar or keel
a low speed as described in 10.3.1.2. block intended for mechanical testing. Test bars or blocks are
7.4.3 Sample for Analysis by a Thermal Method: cast separately from the same metal as that used to produce the
7.4.3.1 Break the pin of a disk-shaped sample into pieces of castings.
a suitable mass for use as test portions or use the lugs of a 8.1.6 By agreement with the customer, when large castings
probe sample. Analyze a representative number of test portions or large numbers of castings are produced, two or more
to obtain an average value. samples should be obtained.
7.4.3.2 Alternatively, crush the pin or lugs using a percus- 8.1.7 Special considerations apply to the sampling and
sion mortar to obtain a sufficient mass of sample of particle size sample preparation of liquid iron for the determination of
approximately 1 mm to 2 mm. Avoid the production of fine hydrogen, oxygen, and nitrogen (see 8.5).
material during crushing. For a slab-shaped sample, break the 8.2 Spoon Sampling:
sample into small pieces and crush the pieces in a similar
8.2.1 General:
manner.
8.2.1.1 Sampling should take place before any additions of
7.4.4 Sample for Analysis by a Spectrochemical Method:
inoculating agents to the melt.
7.4.4.1 In the case of a disk-shaped sample, remove any lugs
or pin, as necessary, and grind the surface of the sample to NOTE 2—When sampling takes place before addition of inoculating
expose a white iron structure that is representative of the agents, recognize that the sample obtained will not be representative of the
chemical composition of the cast product.
sample. The amount of material to be removed in this way
should be determined for the chemical composition of the 8.2.1.2 Alternatively, sufficient time should elapse for the
particular iron, and the conditions of sampling. The thickness immediate effect of the additions to fade and the melt should be
of the layer to be removed is normally 0.5 mm to 1 mm. thoroughly stirred before sampling. Failure to allow adequate
7.4.4.2 For a slab-shaped sample, break the slab into two standing time before taking the sample will seriously impair
pieces to obtain a sample of suitable size. the representivity of sampling.
7.4.4.3 Prepare the surface of the sample by grinding and 8.2.1.3 Ductile iron is difficult to sample due to the possi-
linishing. Grinding should be performed wet to avoid overheat- bility of contamination by dross during the production process.
ing the sample but the final surface preparation should be dry A suitable sample may be obtained by filtering the iron using
linishing. Alternatively, cool the sample after grinding by a ceramic disk.
immersion in water, and then finish by dry linishing. 8.2.2 Methods—A graphite spoon or a steel spoon lined with
7.4.4.4 Particular care is required when preparing the sur- a layer of a refractory, such as ganister, is suitable for use in
face of thin samples. A chuck should be specially designed to accordance with one of the following methods.
hold the sample securely during grinding and linishing opera- 8.2.2.1 Remove any slag from the surface of the melt by
tions. skimming, and then immerse a preheated spoon into the melt
and fill with liquid iron.
8. Liquid Iron for Cast Iron Production 8.2.2.2 Introduce a preheated spoon into the stream during
8.1 General: pouring and fill with liquid iron.
8.1.1 The following methods are applicable to the sampling 8.2.3 Chilled Sample:
of liquid iron from cupola furnaces and electric furnaces, 8.2.3.1 Pour the liquid iron from the spoon without delay
holding furnaces in duplex processes, and ladles and treatment into a split mold made from graphite, hematite iron, or copper
vessels. to obtain a sample in the form of a small, flat plate, 4 mm to
8.1.2 Liquid iron intended for the production of iron cast- 8 mm in thickness. Remove the sample from the mold when
ings may be subject to inhomogeneity and particular care is solidified to avoid overheating the mold and the risk of sample
required in the design of strategies and methods of sampling to breakage. Break off any riser.
meet the requirements of the particular production process. For 8.2.3.2 The sample, commonly described as a coin sample,
example, liquid iron in holding furnaces tends to stratify, and may be circular, rectangular, or square with typical sizes,
sampling should ensure that analysis is representative of the respectively, 35-mm to 40-mm diameter, (50 by 27) mm and
melt as a whole. (50 by 50) mm. Generally, disk samples are cast vertically and
8.1.3 In batch processes, two or more samples should be rectangular and square samples are cast horizontally.
taken from melting furnaces preferably when approximately 8.2.3.3 The mold is constructed in two pieces that are
one third and two thirds of the melt has been discharged and an clamped together in use: one piece is a flat chill plate, and the

7
 E1806 − 23
other is a block with the mold cavity. The edge of the mold using a tungsten-carbide-tipped tool adjusting the speed and
cavity may be tapered to facilitate removal of the sample from feed to produce chips of uniform size avoiding the production
the mold. of fine particles. Avoid overheating the sample and the tool.
8.2.3.4 A coin sample with one or more attached pins can be Chips should be as solid and compact as possible with a mass
obtained using a combination-type mold. The pins are broken of approximately 10 mg to prevent crumbling and loss of
off from the disk and used, if required, as test portions for graphite. Chips should not be cleaned with a solvent or treated
analysis by a thermal method. A vertical mold of this type, magnetically because of the risk of altering the distribution of
commonly described as a book mold and made from low- metal and graphite. A tool with a diameter of 10 mm is suitable
phosphorus, high-carbon grey iron, or from copper or graphite, for use when obtaining chips by drilling.
is shown in Fig. 2. The sample obtained is a disk, 38 mm in 8.4.2.2 The size range of chips intended for the determina-
diameter by 6 mm thick, with three 5-mm diameter pins. tion of total carbon should be 1 mm to 2 mm.
8.2.3.5 The temperature of the liquid iron in the spoon 8.4.2.3 When machining is not practicable, the sample can
should be as high as possible and compatible with the mold be broken into pieces and the pieces crushed using a percussion
material. It is essential that the mold is cold to ensure adequate mortar or vibratory grinding mill to obtain a sufficient mass of
chilling for the production of a sample with a white iron sample of particle size less than 150 µm. Use this method
structure. If necessary, the mold should be air-cooled before where it can be shown that pulverization does not lead to
use. The mold should be free from moisture. contamination of the sample.
8.2.3.6 For processes where samples are required to be 8.4.2.4 For a chilled sample, drill the sample, if practicable,
taken at frequent intervals, provide several molds to ensure the discarding chips obtained from the surface.
availability of a mold that is cold. 8.4.2.5 For a non-chilled sample, like a cylindrical block,
8.2.3.7 Thermal stress due to overheating of the mold can drill a hole transversely at a position one third along the length
cause breakage of the coin sample and should be avoided. of the block. Then drill another hole from the opposite side.
8.2.4 Non-Chilled Sample: Discard chips from one third of the radial depth in both
8.2.4.1 Pour the liquid iron from the spoon without delay directions. Continue drilling through the center of the block to
into a sand mold to obtain a cylindrical block-shaped sample obtain the sample.
approximately 50 mm in diameter by 40 mm to 50 mm long. 8.4.2.6 For a test bar, either grind two flats on opposite sides
8.2.4.2 Alternatively, a sample can be selected from a test of the bar and drill from one side to the other at a position one
bar or keel block intended for mechanical testing. Test bars or third along the bar or turn the test bar using a lathe with a
blocks are cast either from liquid iron taken from a ladle using maximum cut of 0.25 mm. Do not use a cutting fluid or
a pouring spoon, or, if a small hand-ladle is used for pouring, coolant. Use a radial cut from edge to center, or face turn a
directly from the ladle itself. Bars are typically 30 mm in cross section of the bar, but do not confine turning to the
diameter by 150 mm long and may be cast vertically or surface of the bar. Discard chips obtained from the surface of
horizontally in a sand mold. the bar. For a non-machinable sample, break pieces from the
8.2.4.3 Allow samples to cool completely before removal sample or cut a 3-mm slice or disk from the cross section near
from the mold. the bottom of a test bar. Crush these pieces using a percussion
8.2.5 Maintenance of Equipment: mortar or vibratory grinding mill to obtain a sufficient mass of
8.2.5.1 It is essential to maintain pouring spoons and molds sample of particle size less than 150 µm.
in a clean and dry condition. After use, remove any slag and 8.4.3 Sample in the Form of a Solid Mass for Analysis by a
skull and brush the faces of the mold. Thermal Method:
8.2.5.2 Molds should be remachined if the surfaces become 8.4.3.1 For a chilled sample, remove a pin from the sample
worn. This avoids the need for additional machining of the and break or cut the pin into pieces for use as test portions.
sample during surface preparation.
8.4.3.2 Alternatively, crush the pin in a percussion mortar to
8.3 Probe Sampling—Probe sampling has limited use in the provide a sample of particle size range approximately 1 mm to
manufacture of cast iron products. Sampling probes, if 2 mm. Avoid the production of fine material.
required, should be designed to provide samples from the melt 8.4.3.3 For a non-chilled sample, use a saw to cut a 3-mm
of a quality and metallurgical structure required by the analysis disk or slice from the cross section of a cylindrical block or test
method. bar and cut pieces of a suitable mass for use as test portions.
8.4 Preparation of a Sample for Analysis: 8.4.3.4 Analyze a representative number of test portions to
8.4.1 Preliminary Preparation: obtain an average value. The mass of a piece selected as a test
8.4.1.1 Remove any sand adhering to the surface of a portion should not be less than approximately 0.3 g.
sand-cast sample by scratch brushing or shot-blasting. Remove 8.4.4 Sample for Analysis by a Spectrochemical Method:
any surface oxidation by grinding. 8.4.4.1 For a chilled sample, remove any pins and then use
8.4.1.2 Prepare the sample in accordance with one of the a fixed-head grinder to expose a white iron structure which is
following procedures depending upon the method selected for representative of the sample. The amount of material to be
analysis. removed in this way should be determined for the chemical
8.4.2 Sample for Analysis by a Chemical Method: composition of the particular iron and the conditions of
8.4.2.1 Machining to obtain chips should be conducted by sampling. The thickness of the layer to be removed is normally
drilling or turning at a low speed (100 r ⁄min to 150 r ⁄min) at least 1 mm.

8
 E1806 − 23
8.4.4.2 Air-cooling is recommended during grinding. Grind- 9. Liquid Steel for Steel Production
ing can be conducted wet to avoid overheating the sample, but
9.1 General:
the final treatment should be dry grinding or linishing. Exces-
sive grinding may lead to analysis errors if the chill region of 9.1.1 The following methods are applicable to the sampling
the sample is exceeded. Chilled samples should be examined of liquid steel from furnaces, ladles, and other vessels, and
regularly in routine practice to ensure the suitability of the from tundishes and molds during the melting, secondary
metallurgical structure of the prepared sample for the analysis treatment, and casting of the steel.
method. 9.1.2 Special considerations apply to sampling and sample
8.4.4.3 For a non-chilled sample, use a grinding or linishing preparation of liquid steel for the determination of oxygen and
machine to remove a layer approximately 1 mm in thickness hydrogen. See 9.5 and 9.6, respectively.
from the surface of the sample. Air cooling is recommended 9.2 Probe Sampling:
during grinding and, liquid coolants should not be used. 9.2.1 General:
8.4.4.4 For irons that are subject to segregation effects, for 9.2.1.1 The main features of the different types of commer-
example, high-phosphorus engineering iron, high-silicon duc- cially available sampling probes for use with liquid steel are
tile iron, malleable iron, prepare the surfaces of two sides of the distinguished in Annex A1.
sample to obtain an average value. 9.2.1.2 Probe sampling is influenced by such factors as the
8.4.4.5 Avoid overheating of the sample during surface angle and depth of immersion of the sampler and the time of
preparation as this can result in surface crazing that will affect immersion in the melt. It is essential that these factors be
correctness of analysis. determined for the particular conditions of composition and
8.4.4.6 Care is required when preparing the surface of a thin temperature of the steel involved, and thereafter, strictly
coin-sample. A chuck should be designed to hold the sample controlled to maintain the standard of quality required for the
securely during grinding operations. analysis.
NOTE 3—A fixed-head grinder is preferred to a swing grinder for
9.2.1.3 Take precautions to ensure that the operation of
surface preparation; the latter type of equipment may not give a flat probe sampling does not contaminate the sample of liquid steel
surface to the sample. particularly when sampling for the determination of elements
8.5 Sampling and Sample Preparation for the Determina- present in low amounts. The selection of materials used for
tion of Oxygen, Nitrogen, and Hydrogen: construction of the sampling probe, the design of the capping
and entrance system, and the method of deoxidation should be
8.5.1 General—The determination of oxygen, nitrogen, and
such as to minimize risk of contamination, other than from the
hydrogen is required infrequently in the production of castings.
deoxidant itself.
Sampling and sample preparation methods should minimize
hydrogen losses and avoid contamination of the sample by 9.2.2 Procedures:
oxygen, nitrogen, or hydrogen. 9.2.2.1 For sampling from deep melts, such as melting
8.5.2 Procedure: furnaces and ladles, quickly immerse a suitable probe sampler
through the slag layer into the melt as near as possible to the
8.5.2.1 It is essential that a sample for the determination of
center of the melt, at an angle as near as possible to 90°.
hydrogen should be cooled very rapidly. It should be removed
from the mold immediately after solidification and quenched 9.2.2.2 For sampling from shallow melts, such as in
without delay. A mixture of acetone and solid carbon dioxide in tundishes, and from ingot mold tops and continuous casting
the form of a slurry is suitable for quenching. The sample molds, introduce the entry tube of a suitable suction sampling
should be stored by immersion in a refrigerant. probe through the slag or covering powder into the melt. Create
a partial vacuum in the sampler for approximately 2 s to fill the
8.5.2.2 For the determination of oxygen and nitrogen, pins
mold.
broken from a chill-cast sample normally are suitable. Such
9.2.2.3 Some tundishes may contain a sufficient depth of
samples may be obtained from the melt using a spoon, then
liquid metal to permit the use of an immersion sampling probe.
casting the liquid iron as described in 8.2 into a book
combination-type mold to obtain pin-shaped samples of 6 mm 9.2.2.4 For sampling from a stream, introduce a suitable
to 8 mm in diameter. For this purpose, the construction of the stream sampling probe into the metal flow from a ladle, at an
mold shown in Fig. 2 should be modified by enlarging the three angle of 45°, at a position as near as possible to the nozzle of
pin-shaped cavities to produce pins of the required diameter. the ladle. Care should be exercised when inserting the probe
sampler into the stream. It may be necessary to reduce the flow
8.5.3 Preparation of the Test Portion:
of metal during sampling.
8.5.3.1 Remove all traces of surface oxidation from the pin
9.2.2.5 Withdraw the probe sampler from the melt after a
by turning using a lathe and a tungsten-carbide-tipped tool. Use
predetermined interval of time and break it apart. Allow the
a separate parting tool to cut the pin transversely to obtain a test
probe sample to cool somewhat in air, to a dull red color, and
portion of a suitable mass for analysis. Avoid overheating the
then quench in water in a manner that does not cause cracking.
pin during the preparation of test portions for the determination
Sometimes probe samples are transported to the laboratory
of hydrogen, and cool at frequent intervals using crushed, solid
while still hot.
carbon dioxide.
8.5.3.2 There should be no delay between preparation of the 9.3 Spoon Sampling:
test portion and analysis. 9.3.1 Procedures:

9
 E1806 − 23
9.3.1.1 For sampling from the melt, lower the spoon 9.4.3.1 For a probe sample with attached lugs, break off one
through the slag into the melt and fill with liquid steel. The of the lugs to constitute a test portion.
spoon should first be immersed into the slag layer to coat it 9.4.3.2 For a dual-thickness probe sample, punch a slug
with slag so as to reduce chilling and prevent adhesion of the from the thin section of the disk to constitute a test portion.
sample to the spoon. Withdraw the spoon, and remove any slag Heat treatment may be required to soften the probe sample
by skimming the surface of the liquid steel in the spoon. sufficiently for ease of punching if the hardness of the sample
9.3.1.2 For sampling from the stream, introduce the spoon exceeds approximately Rockwell HRC 25.
into the stream from the ladle; fill with liquid steel; then 9.4.3.3 For a disk-and-pin probe sample, from the pin cutoff
withdraw the spoon. a test portion of a suitable mass for analysis.
9.3.1.3 Exercise care when introducing the spoon into the 9.4.3.4 Particular care is required for samples when deter-
stream because of the force of the liquid metal emerging from mining carbon in low-carbon steels to prevent contamination
the nozzle. It may be necessary to reduce the rate of metal flow during preparation of the test portion. Use tweezers for all
during the sampling operation. manipulations.
9.3.1.4 If necessary, add a measured quantity of deoxidant 9.4.4 Sample for Analysis by a Spectrochemical Method:
to the liquid steel in the spoon. When the liquid steel is 9.4.4.1 For a spoon sample, cut off the base of the cylindri-
quiescent (after an interval of up to 10 s), pour without cal sample, using an abrasive cutting-off disk to constitute the
interruption into a one-piece steel mold designed to produce a sample for analysis, usually 20 mm to 30 mm in thickness.
tapered cylindrical sample. The dimensions of the sample Linish the cut surface before analysis.
should be approximately 25 mm to 40 mm in diameter at the 9.4.4.2 For a probe sample, remove any lugs or pin, as
top and 20 mm to 35 mm in diameter at the base, and 40 mm necessary, and then mill or linish the surface of the disk to
to 75 mm long. expose a surface representative of the sample. The amount of
NOTE 4—Aluminum wire is frequently used as the deoxidant in spoon
material to be removed should be determined for the chemical
sampling provided that aluminum does not cause interference in the composition of the particular steel and the conditions of
analysis method and that the determination of the aluminum content of the sampling. The thickness of the layer to be removed normally
melt is not required. The amount of aluminum added is usually between lies between 1 mm and 2 mm. For a dual-thickness probe
0.1 % (m ⁄m) and 0.2 % (m ⁄m). Other deoxidants, such as, titanium or sample, prepare the thick section of the disk.
zirconium, can be used with similar restrictions.
9.4.4.3 For samples of leaded steels, enclose equipment
9.3.1.5 Remove the sample from the mold and cool in a used for surface preparation and fit it with dust extraction
manner to prevent cracking and to ensure ease of machining. equipment. (Warning—Swarf arising from the surface prepa-
9.3.1.6 For sampling stainless steel, a refractory ring placed ration of leaded-steels, and dust from dust extraction filter
on a cast iron plate may be used as a mold. The ring should systems, shall be collected and disposed of safely in accor-
have a wall thickness of 10 mm to 12 mm. The sample is dance with local regulations for lead-containing waste materi-
removed from the mold by breaking off the refractory. als.)
9.3.2 Maintenance of Equipment:
9.5 Sampling and Sample Preparation for the Determina-
9.3.2.1 Maintain sampling spoons and metal molds in a
tion of Oxygen:
clean and dry condition.
9.5.1 Methods of Sampling:
9.3.2.2 Molds should be remachined if the internal surfaces
9.5.1.1 Methods of sampling liquid steel for the determina-
become worn. This avoids the need for additional machining of
tion of oxygen are based upon the use of commercially
the sample during surface preparation. After use, remove any
available sampling probes. The main features of the different
slag and skull from the mold, and clean the surfaces with a wire
types of probes are distinguished in Annex A1. Methods of use
brush.
should be designed to ensure that the operation of sampling
9.4 Preparation of a Sample for Analysis: does not influence the equilibrium between carbon and oxygen
9.4.1 Preliminary Preparation—From a sample taken from in the melt. It is essential to avoid contamination of the sample
the melt, remove any surface oxidation that may contaminate and to remove all surface oxidation at each stage in sample
the sample during subsequent preparation. preparation.
9.4.2 Sample for Analysis by a Chemical Method: 9.5.1.2 Small appendages to probe samples, such as a pin or
9.4.2.1 For a spoon sample, drill the cylindrical sample at a a lug, generally are not suitable for preparation as a test portion
point one third from the bottom through to the center of the free from surface oxidation. A slug obtained by punching from
sample, discarding the chips obtained from the surface layer of a dual thickness probe sample may be satisfactory. For some
the sample. Alternatively, remove the bottom third of the applications, it may be preferred to obtain a sample of larger
cylindrical sample using a cutting-off machine and mill across mass by using a sampling probe filled by gravity.
the whole of the exposed face of the remainder. Heat treatment 9.5.2 Preparation of the Test Portion:
may be necessary to soften the sample sufficiently for machin- 9.5.2.1 Remove oxidation products from the surface of the
ing. probe sample by abrasion in a manner that does not cause
9.4.2.2 For a probe sample, obtain chips from the disk overheating.
section of the sample by drilling or milling as described in 9.5.2.2 Cut a slice from the disk of a probe sample, then cut
11.2.2. a cube-shaped test portion from this slice of a mass suitable for
9.4.3 Sample for Analysis by a Thermal Method: analysis.

10
 E1806 − 23
9.5.2.3 Place the test portion in a stainless steel holding varying diameter is available (see Annex A2). Use the selected
block or some other device to hold it firmly and abrade each sampling probe in accordance with the manufacturer’s guid-
surface using a fine-cut file or abrade all surfaces with ance.
water-cooled silicon-carbide abrasive media. Use tweezers for 9.6.2.2 It is essential that the probe sample be quenched in
all manipulations. ice water and that the ice water be stirred vigorously and
9.5.2.4 Immerse the test portion in acetone and dry in air or continuously during quenching. There should be no delay, and
by exposure to a rough vacuum. Analyze immediately. There quenching should take place within an interval not greater than
should be no delay between preparation of the test portion and 10 s after taking the sample. To allow rapid cooling, quickly
analysis. remove the silica sheath around the sample mold.
9.6.2.3 When the sample is sufficiently cooled, immerse the
9.6 Sampling and Sample Preparation for the Determina-
probe sample in a refrigerant for storage and transport to the
tion of Hydrogen:
laboratory.
9.6.1 General:
9.6.2.4 If the probe is designed to capture diffusible
9.6.1.1 Methods of sampling liquid steel for the determina- hydrogen, quench it to cool sufficiently for handling purposes.
tion of hydrogen are based upon the use of commercial 9.6.3 Preparation of the Test Portion:
sampling probes. The main features of the different types of
9.6.3.1 Cut a test portion of a suitable mass for analysis
probes are distinguished in Annex A2. Methods of use should
from the central sections of the probe sample. Cutting should
minimize and control the rapid diffusion of hydrogen from the
be conducted in such a manner to minimize heating the probe
probe sample that occurs during storage and preparation of the
sample. Use a copious flow of cooling fluid during cutting or
test portion. Losses by diffusion may be large at ambient
cool the sample at frequent intervals, or use a combination of
temperatures especially from small-diameter samples.
both methods of cooling.
9.6.1.2 The probe sample should be free from cracks and
surface porosity, and from moisture, particularly entrapped NOTE 5—Cutting without heating the sample can be accomplished by
water. The condition of the test portion can strongly influence rapidly breaking pieces from the probe sample with manual or hydraulic
bolt cutters.
the analytical measurement. Methods of analysis may differ in
their sensitivity to the presence of water in the sample. If a 9.6.3.2 Prepare the surface of the test portion by filing, grit
suction sampling probe is used, the method of operation should blasting, acid etching, or light grinding. If filing is used, abrade
avoid risk of introduction of moisture into the sample. the surface by hand with a fine-cut file. If grit blasting is used,
9.6.1.3 The choice of a method of sampling is dependent on a grit-blasting machine should be reserved exclusively for this
the temperature of the melt, the method of analysis, and the purpose to avoid contamination from the grit. If grinding is
analytical precision required. These relationships should be used, cool the test portion at frequent intervals. It is difficult to
investigated to establish a suitable method for a particular prevent the sample from being heated with any of these surface
steel-making practice that will give samples of the quality preparation methods. If the test portion is of good quality, no
required. Procedural detail should be rigidly followed to obtain surface preparation using any of these methods should be
consistency in the quality of analysis. necessary.
9.6.1.4 It is essential to maintain the probe sample and the 9.6.3.3 Degrease the test portion by immersion in acetone,
test portion at a temperature that is as low as possible at all dry by exposure to a rough vacuum, and analyze immediately.
stages following sampling, and during storage and sample Alternatively, prepare the test portion by immersion in
preparation. The sample should be stored in a refrigerant. propanol-2 (isopropyl alcohol), and then dry it with diethyl
Liquefied nitrogen or a mixture of acetone and solid carbon ether.
dioxide in the form of a slurry are suitable.
9.6.1.5 The probe sample and the test portion should be kept 10. Pig Irons
cold when cutting the sample and during preparation of the test 10.1 General:
portion. Cooling may be performed by immersion in water that 10.1.1 The following methods are applicable to the sam-
is ice-cold or preferably in a refrigerant. Remove any moisture pling of iron from the blast furnace that has been cast into
present on the surface of the test portion after cooling; immerse pieces of a simple shape, known as a pig, usually in the form
the test portion in acetone; then dry by exposure to a rough of a double lozenge or some other similar shape. The various
vacuum for a few seconds. types of pig irons are classified in ISO 9147. Other types of
9.6.1.6 Discard samples that have been cooled or stored iron may be used in the manufacture of cast iron, for example,
inadequately. iron produced in a cupola furnace or an electric melting
9.6.1.7 Preparation of the surface of the test portion by furnace.
abrading should be kept to a minimum consistent with the need 10.1.2 Use special care to ensure the collection of a repre-
to remove all oxidation products and surface defects. sentative sample from pig irons.
9.6.1.8 Analyze the test portion immediately after prepara- 10.2 Increment Sampling:
tion. 10.2.1 Number of Increments—Ensure that the number of
9.6.2 Methods of Sampling: pigs taken as incremental samples are representative of the
9.6.2.1 A range of commercially available sampling probes batch or consignment. For a consignment supplied in bulk, if
designed to provide pin-shaped or pencil-shaped samples of there is no other agreement between the supplier and the

11
 E1806 − 23
purchaser, the minimum number of pigs taken from a consign- 10.3.1.3 For some types of iron, (for example, oxygen-
ment shall be in accordance with ISO 9147 (see Table 1). blown iron), it may be necessary to use a tungsten-carbide-
10.2.2 Methods: tipped tool.
10.2.2.1 During unloading or loading operations, or any 10.3.1.4 Chips should be as solid and compact as possible to
other displacement of a consignment, obtain pigs as incremen- prevent crumbling and loss of graphite. The particle size range
tal samples at intervals of time or mass that are approximately of chips intended for the determination of carbon should be
equal. approximately 1 mm to 2 mm.
10.2.2.2 For a consignment supplied in wagons or trucks, 10.3.1.5 Do not employ milling because of the high propor-
the points of sampling shall be prescribed in a definite order, tion of fines produced.
for example, from five positions, one at the center of the wagon 10.3.1.6 Do not rinse the prepared sample with a solvent or
and four others at one sixth of the distance from each of the treat it magnetically because of the risk of altering the
corners of the wagons along the two diagonals. distribution of metal and graphite.
10.2.2.3 For a stockpile, throw a rope having a certain 10.3.2 Sample for Analysis by a Chemical Method—Prepare
number of knots onto the pile, and take the pigs touched by each of the incremental samples using one of the following
these knots. Repeat the operation until a sufficient number of methods:
pigs is obtained. 10.3.2.1 For machinable iron, clean one face of the pig by
10.2.2.4 Where it is not possible to gain access to the whole grinding at a position midway along the length and width to
of the surface of the stockpile, or where access to the stockpile expose an area of metallic surface of at least 50 mm in
is unsafe, the points of sampling shall be prescribed in a diameter. Drill a hole through the cross section of the pig, and
definite order on the surface of the stockpile. cease drilling at a point approximately 5 mm from the opposite
10.2.2.5 Alternatively, use a mechanical shovel to obtain a face. If necessary drill an additional hole parallel to the first
number of subsamples from positions in the stockpile selected hole. (See Fig. 3(a), Fig. 3(b), Fig. 3(c), and Fig. 3(d).)
at random. Select one pig at random from each subsample. 10.3.2.2 For non-machinable iron, break the pig at a posi-
10.2.3 Consignment of Mixed Pig Irons: tion midway along its length. Break off pieces from the
10.2.3.1 A consignment of pig iron may contain a number of fractured face; crush these pieces to a particle size of approxi-
different batches of pig iron that may be from different sources. mately 5 mm; then grind using a vibratory grinding mill to a
If pigs of different shapes and sizes can be distinguished in the particle size of less than 150 µm.
consignment, a visual assessment should be made of the 10.3.2.3 Mix equal quantities of the material obtained from
proportions of each type of pig iron present. each pig. From this mixture obtain a sample of sufficient mass
10.2.3.2 Incremental samples should then be taken of each for analysis by coning and quartering.
type of pig iron in the consignment to constitute separate
10.3.2.4 Alternatively, analyze the material obtained from
subsamples of pigs to obtain a weighted average analysis for
each pig separately to obtain an average value for the consign-
the consignment.
ment.
10.3 Preparation of a Sample for Analysis: 10.3.3 Sample for Analysis by a Thermal Method:
10.3.1 General: 10.3.3.1 To prepare samples in the form of chips or frag-
10.3.1.1 If the pigs taken as incremental samples contain ments from machinable iron, at the center of each pig, and on
remnant magnetism as a result of handling with magnetic opposite faces, drill a hole 12 mm to 14 mm in diameter.
grabs, demagnetize them using a demagnetizing coil to prevent Remove scale and any other impurities around the holes on
separation of coarse and fine particles during drilling. both sides of the pig. Then drill another hole coaxial with the
10.3.1.2 To obtain chips by machining, drill at a low speed first hole, 20 mm to 24 mm in diameter, so that large chips,
(100 r ⁄min to 150 r ⁄min) using a freshly sharpened tool and approximately 1 mm to 2 mm in size, are obtained.
adjust the speed and feed to produce chips of uniform size with 10.3.3.2 To prepare samples in the form of chips or frag-
a minimum of fine material. A tool with a diameter of 12 mm ments from non-machinable iron, obtain small pieces from the
to 14 mm is suitable for obtaining chips. Resharpen the tool at pig as described in 7.4.2.1, and then crush these pieces using a
frequent intervals and avoid overheating both the sample and percussion mortar to a particle size between approximately
the tool. 1 mm and 2 mm.
10.3.3.3 Mix equal quantities of the material obtained from
each pig. From this mixture obtain a sample for analysis by
TABLE 1 Minimum Number of Pigs Taken as Incremental coning and quartering.
Samples from a Consignment of Pig Iron 10.3.3.4 Alternatively, analyze the material obtained from
Consignment, Tons Number of Pigs each pig separately to obtain an average value for the consign-
< 10 9 ment.
10–20 11 10.3.3.5 To prepare samples in the form of a solid mass, cut
20–40 12
40–80 14 a slice, approximately 3 mm thick, from the complete cross
80–160 16 section of the pig at a position midway along its length and
160–300 18 clean the edges by grinding. From this slice, cut pieces at
300–600 21
> 600 24 positions corresponding to those shown in Fig. 3(e) or Fig. 3(f)
to constitute test portions of a mass suitable for analysis.

12
 E1806 − 23

FIG. 3 Sampling Positions for Pig Irons

Alternatively, saw or break the pig at a position midway along 11.2.1.1 Sample and prepare samples in accordance with the
its length. Using a trepanning tool, drill either three or five grade of iron, type of casting, and the method selected for
holes at positions corresponding to those shown in Fig. 3(e) analysis.
and Fig. 3(f) to obtain pins of approximately 3 mm in diameter. 11.2.1.2 Clean the sample product or laboratory sample by
Break the pins into pieces to constitute test portions of a mass scratch-brushing, grinding, or shot-blasting to remove adhering
suitable for analysis. particles of sand and to expose areas of metallic surface.
10.3.3.6 Analyze a representative number of the test por- Ensure that both the inner and outer surfaces of hollow castings
tions to obtain an average value for each pig. are clean.
11.2.2 Sample for Analysis by a Chemical Method:
11. Cast Iron Products 11.2.2.1 Machine the sample to obtain chips by drilling or
11.1 General: turning at a low speed (100 r ⁄min to 150 r ⁄min) using a
11.1.1 The location and method of taking a laboratory tungsten-carbide-tipped tool, adjusting the speed and feed to
sample from a cast iron product shall be agreed upon between produce chips of uniform size with a minimum amount of fine
the supplier and the purchaser in relation to one of the methods particles. Take care to avoid overheating both the sample and
described in the following paragraphs. the tool. There is a risk of fracture of the tool when using a
11.1.2 The sample can be selected from a test bar or block carbide-tipped drill. If the tool fractures, the chips should be
cast onto the casting for the purpose of mechanical testing. discarded. Milling shall not be employed owing to the high
11.1.3 Take special care to ensure the collection of a proportion of fines produced.
representative sample from cast iron products. There may be 11.2.2.2 Chips should be as solid and compact as possible
differences in chemical composition, particularly in the con- with a mass of approximately 10 mg to prevent crumbling of
tents of carbon, sulphur, phosphorus, manganese, and magne- graphite. Do not rinse chips with a solvent or treat them
sium between the selected sample and that of the casting or magnetically because of the risk of altering the distribution of
castings as a whole. Segregated elements may concentrate metal and graphite. A 10-mm diameter tool is suitable for
towards the upper surfaces of a casting and under cores. These obtaining chips by drilling. The size range of chips intended for
regions should be avoided when selecting a laboratory sample. the determination of carbon or nitrogen should be approxi-
Sectional dimensions and areas of differential heating or mately 1 mm to 2 mm.
cooling require special attention. Careful consideration is 11.2.2.3 When machining is not practical, the sample can be
necessary in the design of sampling strategies for high phos- broken into pieces and the pieces crushed to a particle size of
phorus engineering iron, and malleable and ductile irons. Pay less than 150 µm using a percussion mortar or a vibratory
particular attention when sampling grey irons to ensure that the grinding mill to obtain a sufficient mass of sample for analysis.
sample is representative of the chemical composition of the Use this method only when it can be shown that pulverization
product especially where segregation is suspected. does not lead to contamination of the sample.
11.1.4 Samples obtained from cast iron products that con- 11.2.2.4 For grey irons, obtain chips from the central section
tain free graphite may not be suitable for accurate analysis by of a casting, that is, from a region that represents approxi-
using spark atomic emission or X-ray fluorescence spectromet- mately one third of a complete section of the casting. Do not
ric methods. For these, it is preferable to use other methods of use chips obtained from the as-cast surface. Where possible
analysis, obtaining suitable samples as described in 11.2.2 and and depending upon the shape of the casting, obtain the chips
11.2.3. by drilling the casting at several positions. Mix chips obtained
11.2 Sampling and Sample Preparation: in this way to constitute the sample for analysis. For a casting
11.2.1 General: of large section, it may be impractical to drill through the

13
 E1806 − 23
casting. For this, drill halfway through the section of the 12. Steel Products
casting. For a hollow casting, such as a pipe, drill completely 12.1 General:
through the wall of the pipe at each end, and in the middle, with 12.1.1 The location and method of selecting a laboratory
the axes of the three drill holes at 120° to each other. For a large sample from a sample product shall be agreed upon between
casting, obtain a laboratory sample of 3 mm to 5 mm in the purchaser and the supplier using one of the methods in the
diameter by using a trepanning tool. Break the sample into following paragraphs.
small pieces and crush pieces to a particle size less than 12.1.2 The laboratory sample can be taken from the sample
150 µm using a percussion mortar or vibratory grinding mill to product at the location indicated in the product standard for the
obtain a sufficient mass of sample. selection of material for mechanical testing. See also
11.2.2.5 For malleable irons, wherever possible, obtain the ISO 14284.
sample prior to treatment by annealing. Annealing causes 12.1.3 Special considerations apply to the sampling and
major segregation. It is essential that a sample taken from an sample preparation of leaded steel products (12.5), and of steel
annealed casting represents the full cross section of a casting. products for the determination of oxygen (12.6), and hydrogen
Particular care is required in obtaining a sample from a casting (12.7).
with variable sectional thickness. If annealed material must be
12.2 Selection of a Laboratory Sample from a Cast Product:
analyzed, remove a complete cross section by machining;
12.2.1 From a cast product of large section, obtain a sample
break into pieces; crush in a percussion mortar or disk mill.
in the form of chips at a point midway between the outside and
Separate the coarse and fine fractions using a 150-µm sieve,
center of the section by drilling parallel to the axis. If this is not
and determine the mass of each fraction. Thoroughly mix each
practical, obtain the sample by drilling the section from the
of the fractions separately and weigh proportionate amounts to
side and collecting chips that represent the part of the section
obtain a representative sample for analysis.
midway between the outside and center.
NOTE 6—Malleable iron products are particularly susceptible to segre- 12.2.2 Alternatively, and where a sample is required in the
gation of manganese sulfide where the manganese to sulfur ratio exceeds form of a solid mass, cut a laboratory sample from the product
2:1. by machining or by using a cutting torch at the half or quarter
11.2.2.6 For white irons and alloy irons, it may be possible cross section of the product.
to obtain the sample by drilling as described in 11.2.2.4. Where 12.3 Selection of a Laboratory Sample from a Wrought
drilling is impractical, cut thin slices from the sample product Product:
or laboratory sample, preferably complete cross sections, using 12.3.1 General:
a saw, or if necessary, an abrasive cutting disk. If an abrasive 12.3.1.1 For a rolled product, conduct the process of select-
cutting disk is used, remove any heat-affected zone. Break the ing a laboratory sample on a section of the product perpen-
slices into pieces and crush in a percussion mortar or vibratory dicular to the direction of rolling and at one end of the product.
grinding mill to a particle size less than 150 µm. Obtain a 12.3.1.2 Methods of obtaining a sample for analysis in the
sufficient mass of sample for analysis. form of a solid mass or chips are illustrated in the following by
11.2.3 Sample in the Form of a Solid Mass for Analysis by reference to products of differing cross sections.
Thermal Methods: 12.3.2 Sections:
11.2.3.1 Cut a thin slice from the sample product or labo- 12.3.2.1 Cut a laboratory sample from the sample product
ratory sample as described in 11.2. transversely in the form of a slice.
11.2.3.2 For a large casting, obtain a sample for analysis of 12.3.2.2 To obtain a sample in the form of a solid mass, cut
3 mm to 5 mm in diameter by using a trepanning tool. Break a piece from the laboratory sample of a suitable size for the
off pieces from the sample or cut using a saw to obtain a analysis method.
number of test portions of suitable mass for analysis. Analyze 12.3.2.3 To obtain a sample in the form of chips, mill the
a representative number of pieces and obtain an average value. whole of the cross-sectional area of the laboratory sample.
The mass of a piece selected as a test portion should not be less Where milling is impractical, drilling may be employed but is
than 0.3 g. not recommended for rimming steels. The most suitable
11.2.4 Sample for Analysis by a Spectrochemical Method: drilling position depends on the shape of the section as follows:
11.2.4.1 Use a saw or abrasive cutting disk to cut a sample 12.3.2.4 For a section of symmetrical shape, (for example, a
of suitable size from the sample product or laboratory sample. billet, a round, a slab) obtain chips by drilling a cross-sectional
11.2.4.2 Prepare a cut surface by grinding using a fixed- cut face in a direction parallel to the longitudinal axis at points
head machine or by linishing, or by a combination of both midway between the center and edges (see Fig. 4(a) and Fig.
methods. Air cool the sample to avoid overheating. Do not use 4(b)).
liquid coolants. 12.3.2.5 For a section of complex shape, for example, an
angle, a tee, a channel, or a beam, obtain chips by drilling at
NOTE 7—A fixed-head grinder is preferred to a swing grinder for points indicated in Fig. 4(c), Fig. 4(d), Fig. 4(e), Fig. 4(f), and
surface preparation, the latter type of equipment may not produce a flat Fig. 4(g) leaving a clearance of at least 1 mm around the drill.
surface on the sample for analysis.
12.3.2.6 For a rail, obtain chips by drilling a hole, 20-mm to
11.2.4.3 The method selected for remelting should produce 25-mm diameter in the head of the rail at a position halfway
a chill cast sample with a white iron structure. Take care to between the centerline and edge of the rail (see Fig. 4(h) and
avoid partial losses of elements. Fig. 4(j)).

14
 E1806 − 23

FIG. 4 Sampling Positions for Steel Sections

12.3.2.7 Where drilling into the end or cut face of the either by bundling the material after cutting into suitable
section is impractical, obtain chips by drilling inwards from the lengths, or by folding.
surface perpendicular to the main axis. 12.3.4.3 For a sheet or a strip where the rolling direction is
12.3.3 Plates or Slabs—Cut a laboratory sample of a suit- unknown, take lengths of strip in two directions at right angles,
able size for analysis in the form of a solid mass or chips from and combine the resulting samples.
a point midway between the centerline and the outer edge of
12.3.5 Tubes and Pipes—Sampling may be in accordance
the plate. In the example shown in Fig. 4(k), the laboratory
sample is 50 mm wide. Where this is not practical, take the with one of the following methods:
sample from a position agreed upon between the supplier and 12.3.5.1 Cut a laboratory sample at a position 90° from the
the purchaser as being representative of the plate composition. weld on a welded product.
12.3.4 Light Sections, Bars, Rods, Sheets, Strips, and Wires: 12.3.5.2 Cut across the tube and turn or mill across the cut
12.3.4.1 Where the sample product is of sufficient cross- face to obtain a sample in the form of chips. Thin section tubes
sectional area, cut a slice transversely to constitute the labora- may be flattened before milling.
tory sample and obtain a sample for analysis as described in 12.3.5.3 Drill through the wall of the tube or pipe at several
12.3.2. positions around its circumference to obtain a sample in the
12.3.4.2 Where the sample product is of insufficient cross
form of chips.
section for machining, for example, a thin gage sheet, a strip,
or a wire, mill over the combined transverse sections obtained 12.4 Preparation of a Sample:

15
 E1806 − 23
12.4.1 General—Methods for the sample preparation of 12.5.4 Enclose the equipment used for the surface prepara-
steel products shall be in accordance with the general require- tion of a sample by a spectrochemical method and fit it with
ments specified in 6.4. Special requirements are considered in dust extraction equipment.
the following. 12.6 Sampling and Sample Preparation for the Determina-
12.4.2 Sample in the Form of Chips: tion of Oxygen:
12.4.2.1 Chips obtained by machining shall be of a suffi- 12.6.1 General:
ciently small size to avoid or minimize the need for subsequent 12.6.2 Avoid contamination of the sample and remove any
fragmentation to prepare the sample for analysis. The size of surface oxidation at each stage in sampling and sample
the chips should be such that the mass of individual chips is preparation.
approximately 10 mg (100 chips ⁄g) for unalloyed and low- 12.6.2.1 Do not allow the fingers to come into contact with
alloy steels and approximately 2.5 mg (400 chips ⁄g) for high- the test portion. Use tweezers for manipulation. For steels
alloy steels. If the size of the chips is not sufficiently small for containing very low oxygen contents of approximately
analysis, crush the chips in a percussion mortar. < 10 µg ⁄g, machine the test portion under the protection of an
12.4.2.2 Machine in such a manner to avoid the production inert gas.
of fine material. For a sample that does contain fine powder, 12.6.3 Methods of Sampling—Sample using one of the
that is, particles of size less than approximately 50 µm, following methods:
separate the coarse and the fine particles and determine the 12.6.3.1 Cut a suitably shaped laboratory sample by using a
mass of each size fraction. Weigh proportionate parts of each mechanical or abrasive saw. The sample can, for example, be
fraction to obtain a representative sample for analysis. in the form of a small plate or disk. Using a hand or
12.4.2.3 For a sample for the determination of nitrogen, water-cooled abrasive saw, cut a test portion from this sample
contamination of the chips caused by atmospheric nitriding of of suitable mass for analysis.
fine particles may occur during machining. Obtain the sample 12.6.3.2 Cut a laboratory sample in the form of a slice,
by machining the laboratory sample in such a manner to avoid, 3 mm to 4 mm thick, linish the surfaces of the sample using
as much as possible, the production of particles of a size less 60-grit to 80-grit silicon-carbide abrasive paper and then
than approximately 50 µm and preferably in an argon atmo- abrade by using a burr, a rotary tool with cutting teeth, at a
sphere. speed of approximately 30 000 r ⁄min. The condition of the
12.4.2.4 For a sample for the determination of carbon where surfaces of the sample after preparation should be smooth,
the carbon is present in very small amounts, for example, in metallically bright, and free from defects. Punch a slug from
interstitial free steels, the chips may be subject to contamina- the sample of a suitable mass for analysis to constitute a test
tion from carbonaceous materials present in the atmosphere or portion using a 4-mm to 6-mm diameter punch. Perform the
from other sources. The chips should be stored to prevent punching operation so that the test portion falls into a container
contamination. Alternatively prepare a test portion in a solid that can be closed with a cap or stopper.
form such as a slug obtained by punching. (1) If the surfaces of the sample are linished with water
12.4.3 Sample for Analysis in the Form of a Solid Mass: cooled silicon-carbide abrasive media, no further surface
12.4.3.1 For products of thin section, such as strips or preparation should be necessary before punching slugs for use
sheets, produce test portions for analysis by thermal methods as test portions.
by nibbling small pieces from the edge of the product. 12.6.3.3 Cut a rectangular-shaped laboratory sample, ap-
Alternatively, obtain slugs of 4 mm to 6 mm in thickness by proximately 10-mm section by 100 mm long. Turn the sample
punching. using a lathe at a speed of approximately 1000 r ⁄min to a
12.4.3.2 When using a spark atomic emission spectrometric diameter of approximately 7 mm: continue turning at a con-
method for sample of products with a thickness of approxi- trolled feed rate of approximately (0.1 to 0.15) mm/revolution
mately 1.5 mm or less, it is necessary to reduce the local at a speed of (800 to 1000) r/min to reduce the diameter of the
heating that occurs when the electrical discharge is produced. sample to 6 mm. The condition of the surfaces of the sample
For example, the edges of the sample can be electrically after preparation should be smooth, metallically bright and free
welded to a small block of steel or the sample can be embedded from defects. Do not use cooling lubricants during the final
in another material such as tin, leaving one surface exposed. stage of the machining process. Using a hand saw, cut a test
portion from the turned sample of a suitable mass for analysis.
12.5 Sampling of Leaded Steel: 12.6.4 Preparation of a Test Portion:
12.5.1 Take care to minimize the creation of dust particles 12.6.4.1 Place the test portion on a stainless steel holding
during all sampling and sample preparation operations. block or some other device to hold the test portion firm. Abrade
(Warning—Swarf arising from machining and surface prepa- the surfaces using a fine-cut file.
ration of leaded steels, and dust from dust extraction filter 12.6.4.2 If the test portion was obtained using the method
systems, shall be disposed of safely in accordance with local described in 12.6.3.1, abrade each of the surfaces of the test
regulations for lead-containing waste materials.) portion.
12.5.2 Select a laboratory sample from the sample product 12.6.4.3 If the test portion was obtained using the method
by cutting using a saw. described in 12.6.3.3, the cylindrical surface of the test portion
12.5.3 Obtain chips by milling at a low speed to avoid should be sufficiently smooth to dispense with the need for
overheating the sample and the creation of dust. filing but each of the two end faces should be prepared using

16
 E1806 − 23
a file. Immerse the test portion in acetone and dry in air or by 12.7.1.6 Discard samples that have been cooled or stored
exposure to a rough vacuum; analyze immediately. inadequately.
12.6.4.4 There should be no delay between the preparation 12.7.1.7 Abrading the surface of the test portion should be
of the test portion and the analysis. kept to a minimum consistent with the need to remove
12.7 Sampling and Sample Preparation for the Determina- oxidation products and surface defects.
tion of Hydrogen: 12.7.1.8 Analyze the test portion immediately after prepa-
12.7.1 General: ration.
12.7.1.1 Methods should be designed to minimize and 12.7.2 Methods of Sampling:
control the rapid diffusion of hydrogen from the sample that 12.7.2.1 From a cast product, obtain a sample of a suitable
occurs during sampling, storage of the sample, and preparation size by using a trepanning tool.
of the test portion. The sample should be free from cracks and 12.7.2.2 From a wrought product or a large forging, using a
surface porosity and from moisture. The condition of the test saw or an abrasive cutting disk, obtain a laboratory sample at
portion can strongly influence the analytical measurement. a position mid-width from the product centerline. From the
Methods of analysis may differ in their sensitivity to the laboratory sample, cut a piece of a size suitable for turning
presence of water. using a lathe in order to obtain a sample for analysis.
12.7.1.2 Rigidly adhere to procedural detail in order to 12.7.2.3 Store the sample in a refrigerant.
obtain consistency in the quality of analysis. 12.7.3 Preparation of a Test Portion:
12.7.1.3 Losses of hydrogen from the sample by diffusion 12.7.3.1 From the sample, cut a test portion of a suitable
may be large at ambient temperatures especially from samples mass in such a manner to minimize heating the sample, then
with thin cross sections. Maintain the laboratory sample and cool the sample at frequent intervals.
test portion at a temperature that is as low as possible at all 12.7.3.2 Prepare the surface of the test portion by filing,
stages during sampling, storage, and sample preparation. Store grit-blasting, or light grinding. If filing is used, abrade the
the sample in a refrigerant; either liquid nitrogen or a slurry of surface by hand with a fine-cut file. If grit-blasting is used, a
acetone and solid carbon dioxide is suitable. blasting machine should be reserved exclusively for this
12.7.1.4 Keep the sample and the test portion cold when purpose to avoid contamination of the test portion from
cutting the sample and during preparation of the test portion. contaminated grit. If grinding is used, cool the test portion at
Either use a copious flow of cooling fluid during all machining frequent intervals. It is difficult to prevent the sample from
operations or cool the sample and test portion at frequent being heated with any of these surface preparation methods. If
intervals, or use a combination of both methods. Cool by the test portion is of good quality, no surface preparation using
immersion in ice-cold water or, preferably, in a refrigerant. any of these methods should be necessary.
Pack samples of large section with solid carbon dioxide in a 12.7.3.3 Degrease the test portion by immersion in acetone,
manner that ensures good thermal contact between the sample dry by exposure to a rough vacuum for a few seconds, then
and the solid carbon dioxide. During intervals between analyze immediately. Alternatively, prepare the test portion for
machining, return rough-cut pieces to storage in a refrigerant. analysis by immersion in propanol-2 (isopropyl alcohol), and
12.7.1.5 Remove any moisture present on the surface of the then dry it with diethyl ether.
test portion after cooling. Immerse the test portion in acetone
and then dry it by exposure to a rough vacuum for a few 13. Keywords
seconds. 13.1 castings; iron sample; sample lot; steel sample

ANNEXES

(Mandatory Information)

A1. SAMPLING PROBES FOR USE WITH LIQUID IRON AND STEEL

A1.1 General A1.1.2 A range of different types of sampling probes is

A1.1.1 Disposable probes for taking samples from liquid available commercially. The main features are described in the
iron and steel consist of a small mold made from pressed steel, following paragraphs with illustrative examples shown in Figs.
ceramic material, or silica tubing, and which are mounted in a A1.1-A1.6. The dimensions given in this annex are for ex-
thick-walled protective cardboard tube. ample only.

17
 E1806 − 23
A1.2.4 Some types of probe combine a thermocouple in a
silica tube adjacent to the sample chamber for measurement of
temperature. Where a measurement sublance is used in a basic
oxygen converter furnace, a mold assembly can be incorpo-
rated with the measurement sensors in the sublance to obtain a
sample for laboratory analysis.
A1.2.5 Probes in which the sample chamber is filled by
ferrostatic pressure consist of a steel split mold held in a
cardboard tube by a collar of refractory material. The mold has
a bottom-entry silica tube with a protective cap of thin steel to
prevent ingress of slag and any other contaminant. Cardboard
tubes, which vary in length from 200 mm to 1500 mm or
longer, may be coated partially with refractory material to
minimize splashing during immersion.
A1.2.5.1 This type of probe is used mainly to obtain
samples from liquid steel in furnaces and ladles. Two designs
are shown in Fig. A1.1.
A1.2.6 The samples obtained by using immersion probes
filled by ferrostatic pressure can differ in configuration.
A1.2.6.1 The disk-and-pin probe samples are exemplified in
Fig. A1.2. The disk is suitable for analysis by a spectrochemi-
cal method, and the pin may be used, if required, for analysis
by a thermal method. The disk may be oval or circular or some
other similar shape.
A1.2.6.2 For disk-and-pin probe samples with a number of
lugs attached to the disk, the lugs have a mass of 0.5 g or 1 g,
and may be easily broken off from the disk and can be used, if
required, as test portions in thermal methods of analysis.
A1.2.6.3 The dual-thickness probe samples are illustrated in
Fig. A1.2(b), in which part of the disk is reduced in thickness
and is suitable for the punching of slugs. The slugs are 4 mm
to 6 mm in diameter and are used as test portions in thermal
methods of analysis. The thicker section of the disk of a
dual-thickness probe sample is used for analysis by spectro-
chemical methods. A probe sample with a hardness of greater
than approximately Rockwell 25 HRC may require heat
FIG. A1.1 Examples of Immersion Probes Filled by Ferrostatic
treatment before punching.
Pressure (a) With the Deoxidant in the Sample Chamber and (b) A1.2.7 Probes of the type shown in Fig. A1.3 in which the
with the Deoxidant in a Separate Mixing Chamber
sample chamber is filled by gravity consist of a two-piece or
four-piece steel cylindrical mold that is contained in a refrac-
A1.2 Immersion Sampling Probes tory assembly and attached to a cardboard tube.
A1.2.1 Immersion probes can be inserted into the liquid A1.2.7.1 The mold has a side entrance port that is protected
metal either by hand or by mechanical means using a lance of in some way to prevent ingress of slag. The assembly may be
steel piping fitted into the cardboard tube or attached directly to sleeved with refractory to minimize splashing during immer-
the probe assembly. Immersion times vary depending on the sion; overall length of the assembly and cardboard tube is
design of the probe and the conditions of sampling, in 400 mm to 800 mm. Immersion times are usually 2 s or 3 s.
particular the temperature of the liquid metal, but are normally A1.2.7.2 This type of probe is used in situations where the
between 3 s and 8 s. disk-and-pin type of sample is not satisfactory for analysis. It
A1.2.2 The lance is constructed so that air from the mold is used to obtain samples from liquid iron and steel in ladles
cavity and gases produced during the combustion of cardboard and from liquid steel in ingot molds and continuous casting
can escape easily. A handle bar is incorporated for controlling tundishes. The sample is typically 30 mm in diameter by
the lance during immersion and withdrawal. 70 mm long.
A1.2.3 When sampling from ladles and secondary treatment A1.2.8 Probes of special design are used to obtain samples
vessels, a mechanical system can be used to lower and raise the from liquid iron in the blast-furnace runner and from the
lance. torpedo car and transfer ladle. These probes incorporate chill

18
 E1806 − 23

NOTE 1—All dimensions are in millimetres.

FIG. A1.2 Disk-and-Pin Samples Showing (a) the Basic Design, (b) the Dual-Thickness Variant, and (c) Layer Stratification of the Disk of
the Sample

FIG. A1.4 Example of an Immersion Probe Used for Sampling

Liquid Iron from a Blast Furnace

FIG. A1.3 Example of an Immersion Sampling Probe Filled by to the disk. This type of probe is shown in Fig. A1.4. The disk
Gravity of the sample can vary in thickness from 8 mm to 12 mm and
the pin is typically 4 mm in diameter. Immersion times vary
plates of varying thickness to ensure that the liquid iron of the from 5 s to 9 s depending upon the application.
sample is chilled very rapidly. Two types are illustrated as A1.2.8.2 The second type is a probe designed to eliminate
follows: the risk of drainage of liquid iron when sampling very fluid
A1.2.8.1 The first type is a variant of the probe filled by metals. The side-entry mold has one or more steel chill-plates
ferrostatic pressure (A1.2.6) with a design based on the use of and is held in a sand body attached to a cardboard tube. This
either a thick-walled, steel split mold or steel chill plates to type of probe can combine a separate or linked pin-shaped
provide a disk-and-pin sample with a number of lugs attached mold. The sample is typically 35 mm in diameter with a

19
 E1806 − 23
a plug in a cardboard tube of length 100 mm to 225 mm.
Samples are of the disk-and-pin type.
A1.3.2 Differing designs of mold construction are used for
the sampling of liquid iron.
A1.3.3 Lances for stream sampling probes are designed so
that the probe can be positioned in the metal stream at an angle
of 45°. Some means of supporting the lance may be provided.
Sampling time is usually 2 s.
A1.3.3.1 This type of probe is used to obtain samples from
liquid iron and steel flowing from ladles.
A1.4 Suction Sampling Probes
A1.4.1 Probes of the type shown in Fig. A1.6(b) consist of
a steel split mold held in position by a plug in a cardboard tube,
about 125 mm in length. The mold has an exposed entry tube
of silica with a protective cap to prevent ingress of slag or
casting powder. Air is removed from the mold to create a
partial vacuum by using a hand-operated pump or a
compressed-air venturi pump. Sampling time is usually 2 s.
A1.4.1.1 This type of probe is used to obtain samples from
liquid steel in small furnaces, ingot molds, continuous casting
molds, and tundishes. Samples are of the disk-and-pin type.
A1.5 Deoxidation Systems for Sampling Probes
A1.5.1 Probes used for the sampling of liquid steel that is
oxidized and effervescent contain a deoxidant usually in the
FIG. A1.5 Example of a Sublance Probe Assembly Showing the form of wire or a pellet inserted in the probe in such a manner
Sample Chamber that it becomes uniformly dispersed in the liquid steel. Various
methods are used to incorporate the deoxidant in the probe, for
thickness varying from 4 mm to 12 mm depending on the example:
metallurgical structure required. The optional pin sample is A1.5.1.1 Deoxidant in the sample chamber itself as shown
6 mm in diameter by 45 mm long. in Fig. A1.1(a) and Fig. A1.3.
A1.2.9 Probes of special design are used to obtain samples A1.5.1.2 Deoxidant in the entry tube to the sample chamber:
from liquid steel in a vacuum induction furnace. A1.5.1.3 Deoxidant in a separate chamber. The deoxidant
A1.2.9.1 In one example, the sampling mechanism in the and liquid steel are thoroughly mixed before the steel enters the
form of tube made from a refractory material is located in the sample chamber, as shown in Fig. A1.1(b). Some probes have
furnace charging system and suspended on a wire rope to a second mixing chamber.
permit vertical access to the liquid metal by gravitational A1.5.1.4 Aluminum, zirconium, or titanium are commonly
means. The sample is cylindrical in shape, 35 mm in diameter. used as deoxidants dependent upon the type of liquid metal and
the analytical requirements.
A1.2.10 Measurement sensor assemblies used with
sublances in basic oxygen steelmaking may incorporate molds A1.6 Quality of Sample
for obtaining samples from liquid steel. Molds of the types
described in A1.2.2 may be used both in the cases of a sublance A1.6.1 Apart from the presence of defects and oxides on the
used during oxygen blowing (in-blow operation) and when surfaces of the disk sample, the surface layers of the disk may
oxygen is not being blown (end-blow operation). For an be subject to segregation and the central portion may be porous
in-blow operation a mold of different design can be used to and subject to shrinkage or other thermal effects as shown in
obtain a sample of a rectangular shape, 40 mm by 30 mm and Fig. A1.2(c). Special care is necessary to ensure that proce-
20 mm thick. dures for preparing the surface of the disk for analysis by
A1.2.10.1 A typical assembly, shown in Fig. A1.5 includes spectrochemical methods expose a layer of metal that is
sensors for the measurement of liquidus arrest, temperature and representative of the chemical composition of the sample.
oxygen potential, and incorporates a rectangular-shaped mold A1.6.1.1 It is usually necessary to remove a layer of 1 mm
with a side entry to obtain a sample during the measurement to 2 mm from the surface of a disk sample obtained from liquid
process. steel to expose a part of the sample that is suitable for the
analysis method selected.
A1.3 Stream Sampling Probes A1.6.2 The amount of material removed from the surface of
A1.3.1 Probes of the type shown in Fig. A1.6(a) consist of chill samples taken from liquid iron is determined by the
a steel split mold with an exposed entry tube of silica held by metallurgical structure of the sample that may vary through the

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FIG. A1.6 Examples of (a) Stream Sampling and (b) Suction Sampling Probes

thickness of the disk. The type of sampling probe used and the A1.6.3 In routine practice, probe samples should be exam-
method of preparing the disk sample should be selected to ined regularly to ensure the suitability of the prepared sample
provide a surface structure of either white or grey iron in for the analysis method.
accordance with the requirements of the analysis method.
A1.6.2.1 For a disk sample obtained from liquid iron, it is
usually necessary to remove a layer of thickness approximately
0.5 mm to 1 mm from the surface of the disk sample.

A2. SAMPLING PROBES FOR USE WITH LIQUID STEEL FOR THE DETERMINATION OF HYDROGEN

A2.1 General anti-splash coating. This type of probe is used for taking
samples from liquid steel at temperatures near to the liquidus
A2.1.1 Disposable probes for taking samples from liquid
point of the steel.
steel for the determination of hydrogen usually consist of a
mold made from pressed steel or silica tubing mounted in a A2.2.1.2 Probes of the type shown in Fig. A2.1(b) consist of
thick-walled protective cardboard tube. Probes are designed to an exposed silica tube, 10 mm to 12 mm in internal diameter,
obtain a pin-shaped or pencil-shaped sample, 7 mm to 12 mm held in a cardboard tube. The top end of the tube is open or may
in diameter by 75 mm to 150 mm long, from liquid steel in be covered with aluminum foil. The tube has a side entrance
ladles, ingot molds, and continuous casting tundishes and port covered with aluminum foil. The tube may contain
molds. aluminum wire as a deoxidant, typically a mass of approxi-
mately 0.1 g. This type of probe is used in a wide range of
A2.1.2 Several types of sampling probes are available applications for taking samples from liquid steel.
commercially; the main features of which are described in the
following sections with illustrative examples shown in Fig. A2.3 Suction Sampling Probes
A2.1.
A2.3.1 Types of Probes for Suction Sampling:
A2.1.3 The dimensions given in this annex are for informa- A2.3.1.1 An evacuated probe of the type shown in Fig.
tion only. A2.1(c) consists of a steel sleeve and a sample chamber made
from high-purity iron with an internal diameter of 4 mm. The
A2.2 Immersion-Sampling Probes
probe is mounted in a cardboard tube and sheathed with a
A2.2.1 Two Types of Probes for Immersion Sampling: heat-resistant material. The probe may have a protective slag
A2.2.1.1 Probes of the type shown in Fig. A2.1(a) consist of cap. On immersion in the melt, the fusible cap melts and liquid
a silica tube, 7 mm to 9 mm in internal diameter contained in steel is aspirated into the evacuated sample chamber, which
a protective cardboard tube. The top end of the tube is open and then closes as the metal solidifies, thus sealing the probe.
the bottom end is capped with aluminum foil to prevent ingress Hydrogen, which diffuses from the sample, is captured in the
of contaminants. The cardboard tube is 250 mm or 400 mm in outer evacuated chamber and is measured when the probe is
length depending upon the application and has a refractory inserted into specially designed analytical equipment and the

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FIG. A2.1 Examples of Probes Used for Sampling Liquid Steel for the Determination of Hydrogen: (a) and (b) Immersion Sampling
Probes, (c) an Evacuated Sampling Probe, and (d) a Suction Sampling Probe

probe pierced. Any residual hydrogen remaining in the sample by 75 mm long, with a silica entry tube. The mold is held in a
can be measured separately after removal of the sample cardboard tube by a collar. Air is removed from the mold to
together with the sample chamber. create a partial vacuum by using a compressed air venturi
A2.3.1.2 Probes of the type shown in Fig. A2.1(d) consist of pump.
a pressed steel split mold, 7 mm to 9 mm in internal diameter

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