ASTM E32-21
(Practice)Standard Practices for Sampling Ferroalloys and Steel Additives for Determination of Chemical Composition
Standard Practices for Sampling Ferroalloys and Steel Additives for Determination of Chemical Composition
SIGNIFICANCE AND USE
4.1 These practices for the sampling of ferroalloys and steel additives are intended for use with test methods used to demonstrate compliance with composition specifications. It is assumed that all who use these methods will be trained samplers capable of performing common sampling procedures skillfully and safely.
SCOPE
1.1 These practices include procedures for the sampling of the various ferroalloys and steel additives, either before or after shipment from the plants of the manufacturers. They are designed to give results representative of each lot that will be comparable with the manufacturer's guaranteed analysis for the same lot. For check analysis, the purchaser may use any sampling procedure desired, but the analytical results obtained on such samples shall not be a basis for compliance or rejection, unless the procedure followed is of an accuracy equivalent to that prescribed in these methods.
1.2 In sampling ferroalloys and steel additives, serious errors often occur from contamination of the samples by iron from the sampling appliances. Therefore, special precautions should be observed to avoid this source of error. Metallic iron may be removed with a magnet from nonmagnetic alloys; its estimation in other alloys requires special analytical procedures (Annex A1). To avoid this error, parts of crushers and pulverizing equipment contacting the samples shall be of steel or other material showing a high resistance to abrasion of the type involved.
1.3 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 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.
General Information
- Status
- Published
- Publication Date
- 30-Apr-2021
- Technical Committee
- E01 - Analytical Chemistry for Metals, Ores, and Related Materials
- Drafting Committee
- E01.01 - Iron, Steel, and Ferroalloys
Relations
- Effective Date
- 01-Jan-2020
- Effective Date
- 15-May-2019
- Effective Date
- 15-May-2016
- Effective Date
- 01-Jul-2015
- Effective Date
- 15-May-2015
- Effective Date
- 15-Aug-2014
- Effective Date
- 01-Apr-2014
- Effective Date
- 15-Feb-2014
- Effective Date
- 01-Dec-2013
- Effective Date
- 01-Oct-2013
- Effective Date
- 15-Sep-2011
- Effective Date
- 15-Jun-2011
- Effective Date
- 15-Jan-2011
- Effective Date
- 01-Jul-2010
- Effective Date
- 15-Jan-2010
Overview
ASTM E32-21 is the internationally recognized standard outlining best practices for sampling ferroalloys and steel additives for the purpose of determining chemical composition. Published by ASTM International, this standard ensures that sampling procedures produce results representative of each lot, comparable with the manufacturer’s guaranteed analysis. ASTM E32-21 is intended for use by trained professionals and supports compliance with composition specifications in metallurgy, quality assurance, and materials analysis.
Ferroalloys and steel additives are critical for steelmaking and other metallurgical processes. Their accurate sampling ensures reliable chemical analysis, which is essential for product performance and regulatory compliance. ASTM E32-21 addresses the risk of sample contamination, particularly from iron, and specifies recommended equipment and precautions to obtain uncontaminated, homogeneous samples.
Key Topics
Sampling Procedures: Covers practices for sampling both lump and crushed forms of ferroalloys and steel additives, whether before or after shipment. Procedures are adapted to the various material formats and shipment types.
Representative Sampling: Emphasizes the importance of a sampling method that accurately reflects the chemical composition of an entire lot. Provides guidelines for the selection and reduction of sample sizes for different shipment scales.
Contamination Prevention: Details the precautions necessary to avoid sample contamination, especially from iron introduced by sampling tools and equipment. Strategies such as the removal of metallic iron from nonmagnetic alloys using magnets are included.
Sample Preparation Equipment: Identifies suitable crushers, riffles (Jones dividers), mortars and pestles, and sieves. Recommends abrasion-resistant steels and proper cleaning to limit composition alterations.
Sample Reduction and Handling: Describes mixing, quartering, coning, and riffling techniques to ensure that final analytical samples are homogeneous and suitable for chemical analysis.
Safety and Units: Mandates adherence to appropriate safety, health, and environmental practices, and clarifies that SI units are standard, with inch-pound values provided for reference.
Applications
ASTM E32-21 is widely applied in:
- Metals and Alloy Manufacturing: Ensures that ferroalloys, steel additives, and related intermediate products are sampled consistently for accurate chemical analysis, supporting quality control and specification verification.
- Quality Assurance Laboratories: Enables laboratories to follow standardized practices for sampling and preparing specimens for elemental analysis.
- Material Compliance and Certification: Assists both manufacturers and purchasers in meeting regulatory and contract requirements for composition analysis.
- Research & Development: Supports metallurgical research by providing a structure for reliable sampling of test materials.
- Supply Chain & Procurement: Offers procedures that purchasers can use for check analysis, ensuring fair acceptance or rejection of delivered materials based on standardized sampling accuracy.
Related Standards
ASTM E32-21 is often used in conjunction with several related ASTM standards, including:
- ASTM E11: Specification for Woven Wire Test Sieve Cloth and Test Sieves
- ASTM E135: Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
- ASTM E354: Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron, Nickel, and Cobalt Alloys
By following ASTM E32-21, industry professionals enhance the accuracy and consistency of chemical composition determination, making it a cornerstone standard for anyone involved in the sampling of ferroalloys and steel additives.
Keywords
Sampling ferroalloys, steel additives, chemical composition, ASTM E32-21, sample preparation, contamination prevention, metallurgy standards, quality assurance.
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Frequently Asked Questions
ASTM E32-21 is a standard published by ASTM International. Its full title is "Standard Practices for Sampling Ferroalloys and Steel Additives for Determination of Chemical Composition". This standard covers: SIGNIFICANCE AND USE 4.1 These practices for the sampling of ferroalloys and steel additives are intended for use with test methods used to demonstrate compliance with composition specifications. It is assumed that all who use these methods will be trained samplers capable of performing common sampling procedures skillfully and safely. SCOPE 1.1 These practices include procedures for the sampling of the various ferroalloys and steel additives, either before or after shipment from the plants of the manufacturers. They are designed to give results representative of each lot that will be comparable with the manufacturer's guaranteed analysis for the same lot. For check analysis, the purchaser may use any sampling procedure desired, but the analytical results obtained on such samples shall not be a basis for compliance or rejection, unless the procedure followed is of an accuracy equivalent to that prescribed in these methods. 1.2 In sampling ferroalloys and steel additives, serious errors often occur from contamination of the samples by iron from the sampling appliances. Therefore, special precautions should be observed to avoid this source of error. Metallic iron may be removed with a magnet from nonmagnetic alloys; its estimation in other alloys requires special analytical procedures (Annex A1). To avoid this error, parts of crushers and pulverizing equipment contacting the samples shall be of steel or other material showing a high resistance to abrasion of the type involved. 1.3 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 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.
SIGNIFICANCE AND USE 4.1 These practices for the sampling of ferroalloys and steel additives are intended for use with test methods used to demonstrate compliance with composition specifications. It is assumed that all who use these methods will be trained samplers capable of performing common sampling procedures skillfully and safely. SCOPE 1.1 These practices include procedures for the sampling of the various ferroalloys and steel additives, either before or after shipment from the plants of the manufacturers. They are designed to give results representative of each lot that will be comparable with the manufacturer's guaranteed analysis for the same lot. For check analysis, the purchaser may use any sampling procedure desired, but the analytical results obtained on such samples shall not be a basis for compliance or rejection, unless the procedure followed is of an accuracy equivalent to that prescribed in these methods. 1.2 In sampling ferroalloys and steel additives, serious errors often occur from contamination of the samples by iron from the sampling appliances. Therefore, special precautions should be observed to avoid this source of error. Metallic iron may be removed with a magnet from nonmagnetic alloys; its estimation in other alloys requires special analytical procedures (Annex A1). To avoid this error, parts of crushers and pulverizing equipment contacting the samples shall be of steel or other material showing a high resistance to abrasion of the type involved. 1.3 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 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.
ASTM E32-21 is classified under the following ICS (International Classification for Standards) categories: 77.040.30 - Chemical analysis of metals; 77.100 - Ferroalloys. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM E32-21 has the following relationships with other standards: It is inter standard links to ASTM E135-20, ASTM E135-19, ASTM E135-16, ASTM E135-15a, ASTM E135-15, ASTM E135-14b, ASTM E135-14a, ASTM E135-14, ASTM E135-13a, ASTM E11-13, ASTM E135-11b, ASTM E135-11a, ASTM E135-11, ASTM E135-10b, ASTM E135-10. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM E32-21 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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: E32 − 21
Standard Practices for
Sampling Ferroalloys and Steel Additives for Determination
of Chemical Composition
This standard is issued under the fixed designation E32; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 These practices include procedures for the sampling of 2.1 ASTM Standards:
thevariousferroalloysandsteeladditives,eitherbeforeorafter E11 Specification for Woven Wire Test Sieve Cloth and Test
shipment from the plants of the manufacturers. They are Sieves
designed to give results representative of each lot that will be E135 Terminology Relating to Analytical Chemistry for
comparable with the manufacturer’s guaranteed analysis for Metals, Ores, and Related Materials
the same lot. For check analysis, the purchaser may use any E354 Test Methods for Chemical Analysis of High-
sampling procedure desired, but the analytical results obtained Temperature,Electrical,Magnetic,andOtherSimilarIron,
on such samples shall not be a basis for compliance or Nickel, and Cobalt Alloys
rejection, unless the procedure followed is of an accuracy
3. Terminology
equivalent to that prescribed in these methods.
3.1 For definitions of terms used in these practices, refer to
1.2 In sampling ferroalloys and steel additives, serious
Terminology E135.
errors often occur from contamination of the samples by iron
from the sampling appliances. Therefore, special precautions
4. Significance and Use
should be observed to avoid this source of error. Metallic iron
may be removed with a magnet from nonmagnetic alloys; its 4.1 These practices for the sampling of ferroalloys and steel
additives are intended for use with test methods used to
estimationinotheralloysrequiresspecialanalyticalprocedures
(Annex A1). To avoid this error, parts of crushers and pulver- demonstrate compliance with composition specifications. It is
assumed that all who use these methods will be trained
izing equipment contacting the samples shall be of steel or
other material showing a high resistance to abrasion of the type samplers capable of performing common sampling procedures
involved. skillfully and safely.
1.3 Units—The values stated in SI units are to be regarded
5. Apparatus for Preparing Samples
as standard. The values given in parentheses after SI units are
5.1 The following equipment is required for the preparation
provided for information only and are not considered standard.
of analytical samples of ferroalloys:
1.4 This standard does not purport to address all of the
5.1.1 Crusher—A strongly built jaw crusher capable of
safety concerns, if any, associated with its use. It is the
rapidly crushing 100 mm (4 in.) lumps to sizes 6.4 mm ( ⁄4 in.)
responsibility of the user of this standard to establish appro-
and smaller shall be used. The crushing plates of this machine
priate safety, health, and environmental practices and deter-
shall be made of a hard and abrasion-resistant steel, such as
mine the applicability of regulatory limitations prior to use.
manganesesteeloraproperlyhardenedalloyorhypereutectoid
1.5 This international standard was developed in accor-
carbon steel.
dance with internationally recognized principles on standard-
5.1.2 Roll Crusher—A roll crusher, the rolls of which are
ization established in the Decision on Principles for the
fitted with tires of hardened and tempered chromium steel to
Development of International Standards, Guides and Recom-
avoid iron contamination of the sample, shall be used to reduce
mendations issued by the World Trade Organization Technical
the 6.4 mm ( ⁄4 in.) pieces to a particle size that will pass the
Barriers to Trade (TBT) Committee.
2.00 mm(No.10)sieveandberetainedonthe850 µm(No.20)
sieve.
These practices are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2021. Published May 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1939. Last previous edition approved in 2015 as E32 – 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E0032-21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E32−21
5.1.3 Riffles—Riffles are usually preferable to the use of material and conditions, such as each cast, each carload, each
hand methods for dividing samples. If available, riffles should ladleful, or each binful.
be of the enclosed type to reduce dust losses. Riffle openings
6.2 Division of Samples—In these methods, the term “di-
should be three (3) times greater than the largest size of the
vide”isusedtoindicateadivisionofasampleintotwoormore
material to be divided. This can be accomplished through the
approximately equal parts of similar composition as in riffling.
use of fixed chute riffles or adjustable finger riffles.
5.1.3.1 For fixed chute riffles, the following are example
7. Sampling Spiegeleisen and 15 % Ferrosilicon
sizes that may be used. Riffles with openings of 12.7 mm, 25.4
7.1 Spiegeleisen is generally cast in pigs and shipped in
mm, 50.8 mm, and 76.2 mm ( ⁄2 in., 1 in., 2 in., and 3 in.)
bulk. Since this alloy is very hard and somewhat tough,
should be available: the 12.7 mm ( ⁄2 in.) riffle to be used for
sampling is most accurately and easily accomplished during
samples containing particles up to 3.2 mm ( ⁄8 in.) in size, the
the tapping of the metal from the furnace or during the
25.4 mm (1 in.) riffle for samples containing particles up to 9.6
pig-casting operation by taking small spoonfuls and pouring
mm ( ⁄8 in.), the 50.8 mm (2 in.) for samples containing
themetalquicklyintoatestmolddesignedtosolidifythemetal
particles up to 19.1 mm ( ⁄4 in.), and the 76.2 mm (3 in.) for
quicklyandgiveacleantestpigthatiseasilybroken.Sampling
samples containing particles up to 50.8 mm (2 in.) in size.
ofthemetalinthesolidstateisdifficult,andisbestdoneduring
5.1.3.2 The use of multiple riffles is not approved.
the loading or unloading, except when the material is loaded
5.1.4 Mortar and Pestle—The mortar and pestle shall both
from bins or unloaded by dumping. The procedure, therefore,
be made of properly hardened alloy steel of a kind and grade
may be varied to suit the conditions but shall always conform
designed to resist severe abrasive forces (Note 1). Suitable
to the following requirements:
dimensions of the mortar are 79.4 mm (3 ⁄8 in.) in outside
7.1.1 Sampling at Furnace—The purchaser may arrange
height, 76.2 mm (3 in.) in outside diameter, 39.7 mm (1 ⁄16 in.)
with the manufacturer to have the sampling done at the
in inside diameter, and 60.3 mm (2 ⁄8 in.) in inside depth, the
furnace. If so, each shipment or each cast may constitute a unit
bottom 12.7 mm ( ⁄2 in.) of which shall be rounded. The pestle
sample for analyzing. The sample shall be obtained by collect-
shall be 152 mm (6 in.) in length, 38.1 mm (1 ⁄2 in.) in
ing portions with a spoon from the runner as the metal flows
diameter, and rounded at the bottom. The upper part of the
from the furnace, unless the metal is treated in the runner or
pestle should be slightly softer than the remainder in order to
ladle to change its composition, in which event the portions
decrease the tendency to shatter. Both the mortar and pestle,
shall be taken as the metal flows from the ladle to the pig
after hardening, shall be polished with abrasive paper to
casting machine. Regardless, at least two spoonfuls of metal
remove all scale. The narrow clearance between the pestle and
shall be taken from each ladle, one spoonful while the first
the sides of the mortar reduces the dust loss.
third of a ladleful is flowing into or from the ladle and the
NOTE 1—For example: steel mortars and pestles of the following second while the last third is flowing. Each spoonful shall be
composition, after proper hardening and tempering treatments, have been
taken in a manner to avoid collecting dirt or slag, and the clean
found satisfactory:
metalshallbeimmediatelypouredintoacleanshallowmoldto
Carbon, % 0.60
form a thin chill casting from which small pieces approxi-
Manganese, % 0.25
mately equal in size may be readily broken. When the
Phosphorus, % 0.02
Sulfur, % 0.02
spiegeleisen is cast in sand beds, the molten metal being run
Silicon, % 0.25
from the furnace directly to the casting floor, the samples shall
Chromium, % 1.25
be taken by dipping skimmed molten metal from the runner
Tungsten, % 2.20
Vanadium, % 0.10
trough and pouring it into a small quartered cast-iron button
mold. A sample shall be taken in this manner to represent the
After machining annealed steel of this grade to the usual form and
metal being cast in each pig bed. From the test castings thus
dimensions, each part is heated to between 760 °C and 800 °C, quenched
obtained to represent a shipment, approximately equal portions
in a light, mineral quenching oil and tempered at once. The pestle may be
treated by quenching the lower portion only, the upper portion being
shall be taken and combined to form the sample which shall
permitted to air cool, and then tempering the quenched portion.
have a gross mass of not less than 200 g.The sample shall then
5.1.4.1 Mechanically operated pulverizing equipment such be alternately crushed in a mortar and sieved until it all passes
through a 180 µm (No. 80) sieve. If the sample is to be
as a ring pulverizer may be substituted for the mortar and
pestle, provided suitable tests show that the use of such analyzed by more than one laboratory, it shall be mixed, coned,
and quartered upon glazed paper (Note 2). The sample or
equipment does not affect the composition of a sample of any
material obtained by these methods. samples thus prepared shall be thoroughly mixed, dried for 1 h
at 105 °C to 110 °C, and preserved for analysis in well-
5.1.5 Sieves—The sieves shall conform to Specification
E11. stoppered bottles properly labeled for full identification, in-
cluding the name of the material, the manufacturer, the date,
6. Unit Quantities for Sampling and Analysis the cast or lot number, etc.
6.1 Each shipment, except as otherwise agreed upon by the
NOTE 2—Finished samples are frequently divided into four portions:
one for the purchaser, one for the manufacturer, one for an umpire if
purchaser and the manufacturer, shall constitute a unit for
necessary, and one held in reserve.
sampling and analysis. It is recommended that shipments of
any alloy exceeding 450 Mg (500 tons) be divided into smaller 7.1.2 SamplingSolidForms—When the metal is in the solid
lots for sampling according to some plan best adapted to the state, a gross sample shall first be collected by selecting
E32−21
random pigs or pieces at regular intervals during the loading or may be present. From each of the lumps in the sample, there
unloading. Surface sampling of piles of the material will not shall be broken three small pieces each about 19 mm ( ⁄4 in.) in
give a representative sample. When piles of the material must size, one from each of two opposite surfaces (top and bottom,
be sampled, the pieces shall be selected according to some ifpresent)andonefromthecenter,thethreepiecesconstituting
fixed plan which assures the obtaining of pieces comprising the a partial vertical cross-section of the lump. Alternatively, a
gross sample from uniformly distributed points throughout, a single piece constituting an entire vertical cross section of the
condition requiring the moving of all or many of the pieces in lump may be taken.
the pile. For lots of 45 Mg (50 tons) or larger, 1 pig or piece
8.2.1 The pieces, together with a representative portion of
shall be taken for each 9 Mg (10 tons), and for small lots the
any fines present, shall be combined and crushed to pass a
number of pieces shall be proportionately increased to 10
6.4 mm ( ⁄4 in.) sieve. Not less than 9 kg (20 lb) shall be
pieces for a 9 Mg (10 ton) lot, or 5 pieces for a 0.9 Mg (1 ton)
separated from the crushed sample by riffling and at least a
lot. The various pigs thus collected shall be broken approxi-
quarter portion of this shall be rolled to pass a 2.00 mm (No.
mately in half by any convenient means, and one of the halves
10) sieve. A 170 g to 220 g (6 oz to 8 oz) portion obtained by
of each pig shall be reserved. From the fractured surface of
riffling (a larger amount when more than one sample is
each of these half pigs, an approximately equal portion shall be
required) of the 2.00 mm sample shall then be pulverized to
taken by any suitable means (as by spalling with a heavy
pass a 150 µm (No. 100) sieve. The pulverizing is best done
hammer), care being taken by the sampler to see that these
with the hardened alloy-steel mortar and pestle, or a ring
spalls are not all from the outer edges of the pigs but at least
pulverizer, while sieving frequently to keep the size close to
some are obtained from the central portion, and that none
150 µm and prevent loss of dust. The pulverized sa
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E32 − 15 E32 − 21
Standard Practices for
Sampling Ferroalloys and Steel Additives for Determination
of Chemical Composition
This standard is issued under the fixed designation E32; 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
1.1 These practices include procedures for the sampling of the various ferroalloys and steel additives, either before or after
shipment from the plants of the manufacturers. They are designed to give results representative of each lot that will be comparable
with the manufacturer’s guaranteed analysis for the same lot. For check analysis, the purchaser may use any sampling procedure
he desires, desired, but the analytical results obtained on such samples shall not be a basis for complaintcompliance or rejection,
unless the procedure followed is of an accuracy equivalent to that prescribed in these methods.
1.2 In sampling ferroalloys and steel additives, serious errors often occur from contamination of the samples by iron from the
sampling appliances. Therefore, special precautions should be observed to avoid this source of error. Metallic iron may be removed
with a magnet from nonmagnetic alloys; its estimation in other alloys requires special analytical procedures (Note 1Annex A1).
To avoid this error, parts of crushers and pulverizing equipment contacting the samples shall be of steel or other material showing
a high resistance to abrasion of the type involved.
NOTE 1—Metallic iron in ferrochromium and ferrosilicon may be determined as follows: Transfer 5 g of the sample of alloy to a 150-mL beaker, add 25
mL of HNO (1 + 3), cover, boil 5 min, filter into a 250-mL beaker, and wash with hot water. Add NH OH in slight excess, heat to boiling, filter, and
3 4
wash with hot water. Dissolve the precipitate on the paper with a minimum quantity of hot HCl (1 + 2), wash the filter with hot water, and titrate the iron
by a standard procedure such as that described in Test Method E354.
1.3 Units—The values stated in SI units are to be regarded as the standard. The inch-pound values in parenthesis are given for
information only.given in parentheses after SI units are provided for information only and are not considered standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
These practices are under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibility
of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Dec. 15, 2015May 1, 2021. Published February 2016May 2021. Originally approved in 1939. Last previous edition approved in 20062015 as
ϵ1
E32 – 86 (2006)E32 – 15. . DOI: 10.1520/E0032-15.10.1520/E0032-21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E32 − 21
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E354 Test Methods for Chemical Analysis of High-Temperature, Electrical, Magnetic, and Other Similar Iron, Nickel, and
Cobalt Alloys
3. Terminology
3.1 For definitions of terms used in these practices, refer to Terminology E135.
4. Significance and Use
4.1 These practices for the sampling of ferroalloys and steel additives are primarily intended to test such materials for compliance
with compositionalintended for use with test methods used to demonstrate compliance with composition specifications. It is
assumed that all who use these methods will be trained samplers capable of performing common sampling procedures skillfully
and safely.
5. Apparatus for Preparing Samples
5.1 The following equipment is required for the preparation of analytical samples of ferroalloys:
5.1.1 Crusher—A strongly built jaw crusher capable of rapidly crushing 100-mm (4-in.)100 mm (4 in.) lumps to sizes 6.4 mm ( ⁄4
in.) and smaller shall be used. The crushing plates of this machine shall be made of a hard and abrasion-resistant steel, such as
manganese steel or a properly hardened alloy or hypereutectoid carbon steel.
5.1.2 Roll Crusher—A roll crusher, the rolls of which are fitted with tires of hardened and tempered chromium steel to avoid iron
contamination of the sample, shall be used to reduce the 6.4-mm6.4 mm ( ⁄4-in.) in.) pieces to a particle size that will pass the No.
10 (2.00-mm)2.00 mm (No. 10) sieve and be retained on the No. 20 (850-μm)850 μm (No. 20) sieve.
5.1.3 Riffles—Riffles, also designated as Jones dividers, Riffles are usually preferable to the use of hand methods for dividing
samples. Riffles with openings of 12.7 mm, 25.4 mm, 50.8 mm, and 76.2 mm (If available, riffles ⁄2 in., 1 in., 2 in., and 3 in.)
should be available;should be of the ⁄2-in. riffle to be used for samples containing particles up to 3.2 mm (enclosed type to reduce
dust losses. Riffle openings should be three (3) times greater ⁄8 in.) in size, the 1-in. riffle for samples containing particles up to
9.6 mm (than the largest size of the material to be divided. This can be accomplished through ⁄8 in.), the 2-in. for samples
containing particles up to 19.1 mm (the ⁄4 in.), and the 3-in. for samples containing particles up to 50.8 mm (2 in.) in size. Riffles
should be of the enclosed type to reduce dust losses. The use of multiple riffles is not approved.use of fixed chute riffles or
adjustable finger riffles.
5.1.3.1 For fixed chute riffles, the following are example sizes that may be used. Riffles with openings of 12.7 mm, 25.4 mm, 50.8
1 1
mm, and 76.2 mm ( ⁄2 in., 1 in., 2 in., and 3 in.) should be available: the 12.7 mm ( ⁄2 in.) riffle to be used for samples containing
1 3
particles up to 3.2 mm ( ⁄8 in.) in size, the 25.4 mm (1 in.) riffle for samples containing particles up to 9.6 mm ( ⁄8 in.), the 50.8
mm (2 in.) for samples containing particles up to 19.1 mm ( ⁄4 in.), and the 76.2 mm (3 in.) for samples containing particles up
to 50.8 mm (2 in.) in size.
5.1.3.2 The use of multiple riffles is not approved.
5.1.4 Mortar and Pestle—The mortar and pestle shall both be made of properly hardened alloy steel of a kind and grade designed
to resist severe abrasive forces (Note 21). Suitable dimensions of the mortar are 79.4 mm (3 ⁄8 in.) in outside height, 76.2 mm (3
9 3 1
in.) in outside diameter, 39.7 mm (1 ⁄16 in.) in inside diameter, and 60.3 mm (2 ⁄8 in.) in inside depth, the bottom 12.7 mm ( ⁄2 in.)
of which shall be rounded. The pestle shall be 152 mm (6 in.) in length, 38.1 mm (1 ⁄2 in.) in diameter, and rounded at the bottom.
The upper part of the pestle should be slightly softer than the remainder in order to decrease the tendency to shatter. Both the mortar
and pestle, after hardening, shall be polished with abrasive paper to remove all scale. The narrow clearance between the pestle and
the sides of the mortar reduces the dust loss.
NOTE 1—For example: steel mortars and pestles of the following composition, after proper hardening and tempering treatments, have been found
satisfactory:
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Carbon, % 0.60
Manganese, % 0.25
Phosphorus, % 0.02
Sulfur, % 0.02
Silicon, % 0.25
Chromium, % 1.25
Tungsten, % 2.20
Vanadium, % 0.10
After machining annealed steel of this grade to the usual form and dimensions, each part is heated to between 760 °C and 800 °C, 760 °C and 800 °C,
quenched in a light, mineral quenching oil and tempered at once. The pestle may be treated by quenching the lower portion only, the upper portion being
permitted to air cool, and then tempering the quenched portion.
NOTE 3—Mechanically operated pulverizing equipment such as a ring pulverizer may be substituted for the mortar and pestle, provided suitable tests show
that the use of such equipment does not affect the composition of a sample of any material obtained by these methods.
5.1.4.1 Mechanically operated pulverizing equipment such as a ring pulverizer may be substituted for the mortar and pestle,
provided suitable tests show that the use of such equipment does not affect the composition of a sample of any material obtained
by these methods.
5.1.5 Sieves—The sieves shall conform to Specification E11.
6. Unit Quantities for Sampling and Analysis
6.1 Each shipment, except as otherwise agreed upon by the purchaser and the manufacturer, shall constitute a unit for sampling
and analysis. It is recommended that shipments of any alloy exceeding 450 Mg (500 tons) 450 Mg (500 tons) be divided into
smaller lots for sampling according to some plan best adapted to the material and conditions, such as each cast, each carload, each
ladleful, or each binful.
6.2 Division of Samples—In these methods, the term “divide” is used to indicate a division of a sample into two or more
approximately equal parts of similar composition as in riffling.
7. Sampling Spiegeleisen and 15 % Ferrosilicon
7.1 Spiegeleisen is generally cast in pigs and shipped in bulk. Since this alloy is very hard and somewhat tough, sampling is most
accurately and easily accomplished during the tapping of the metal from the furnace or during the pig-casting operation by taking
small spoonfuls and pouring the metal quickly into a test mold designed to solidify the metal quickly and give a clean test pig that
is easily broken. Sampling of the metal in the solid state is difficult, and is best done during the loading or unloading, except when
the material is loaded from bins or unloaded by dumping. The procedure, therefore, may be varied to suit the conditions but shall
always conform to the following requirements:
7.1.1 Sampling at Furnace—The purchaser may arrange with the manufacturer to have the sampling done at the furnace. If so,
each shipment or each cast may constitute a unit sample for analyzing. The sample shall be obtained by collecting portions with
a spoon from the runner as the metal flows from the furnace, unless the metal is treated in the runner or ladle to change its
composition, in which event the portions shall be taken as the metal flows from the ladle to the pig casting machine. In any case,
Regardless, at least two spoonfuls of metal shall be taken from each ladle, one spoonful while the first third of a ladleful is flowing
into or from the ladle and the second while the last third is flowing. Each spoonful shall be taken in a manner to avoid collecting
dirt or slag, and the clean metal shall be immediately poured into a clean shallow mold to form a thin chill casting from which
small pieces approximately equal in size may be readily broken. When the spiegeleisen is cast in sand beds, the molten metal being
run from the furnace directly to the casting floor, the samples shall be taken by dipping skimmed molten metal from the runner
trough and pouring it into a small quartered cast-iron button mold. A sample shall be taken in this manner to represent the metal
being cast in each pig bed. From the test castings thus obtained to represent a shipment, approximately equal portions shall be taken
and combined to form the sample which shall have a gross mass of not less than 200 g. The sample shall then be alternately crushed
in a mortar and sieved until it all passes through a No. 80 (180-μm)180 μm (No. 80) sieve. If the sample is to be analyzed by more
than one laboratory, it shall be mixed, coned, and quartered upon glazed paper (Note 42). The sample or samples thus prepared
shall be thoroughly mixed, dried for 1 h at 105 °C to 110 °C, 1 h at 105 °C to 110 °C, and preserved for analysis in well-stoppered
bottles properly labeled for full identification, including the name of the material, the manufacturer, the date, the cast or lot number,
etc.
NOTE 2—Finished samples are frequently divided into four portions: one for the purchaser, one for the manufacturer, one for an umpire if necessary, and
one held in reserve.
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7.1.2 Sampling Solid Forms—When the metal is in the solid state, a gross sample shall first be collected by selecting random pigs
or pieces at regular intervals during the loading or unloading. Surface sampling of piles of the material will not give a
representative sample. When piles of the material must be sampled, the pieces shall be selected according to some fixed plan which
assures the obtaining of pieces comprising the gross sample from uniformly distributed points throughout, a condition requiring
the moving of all or many of the pieces in the pile. For lots of 45 Mg (50 tons) or larger, 1 pig or piece shall be taken for each
9 Mg (10 tons), and for small lots the number of pieces shall be proportionately increased to 10 pieces for a 9-Mg (10-ton)9 Mg
(10 ton) lot, or 5 pieces for a 0.9-Mg (1-ton)0.9 Mg (1 ton) lot. The various pigs thus collected shall be broken approximately in
half by any convenient means, and one of the halves of each pig shall be reserved. From the fractured surface of each of these half
pigs, an approximately equal portion shall be taken by any suitable means (as by spalling with a heavy hammer), care being taken
by the sampler to see that these spalls are not all from the outer edges of the pigs but at least some are obtained from the central
portion, and that none contains portions of the outer surface which may be contaminated with sand or other foreign material. The
spallings from each half pig as collected shall be placed in separate envelopes and weighed to the nearest 1 g. 1 g. Each portion
so selected shall be of approximately the same mass.
7.1.2.1 The portions shall then be combined to form the sample and alternately crushed (preferably in a hardened-alloy steel
mortar) and sieved until it passes a No. 6 (3.35-mm)3.35 mm (No. 6) sieve. Between 280 g and 420 g (10 oz and 15 oz) shall then
be se
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