ASTM E32-86(2006)e1
(Practice)Standard Practices for Sampling Ferroalloys and Steel Additives for Determination of Chemical Composition (Withdrawn 2015)
Standard Practices for Sampling Ferroalloys and Steel Additives for Determination of Chemical Composition (Withdrawn 2015)
SIGNIFICANCE AND USE
These practices for the sampling of metals and alloys are primarily intended to test such materials for compliance with compositional 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 he desires, but the analytical results obtained on such samples shall not be a basis for complaint 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 0). 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 0Metallic 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 HNO3 (1 + 3), cover, boil 5 min, filter into a 250-mL beaker, and wash with hot water. Add NH4OH in slight excess, heat to boiling, filter, and 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 E 354.
1.3 The values stated in SI units are to be regarded as the standard. The inch-pound values in parenthesis are given for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
These practices included procedures for the sampling of the various ferroalloys and steel additives, either before or after shipment from the plants of the manufacturers.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, these practices were withdrawn in January 2015 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: E32 − 86(Reapproved 2006)
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.
´ NOTE—Updated Section 2, Referenced Documents in December 2006.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 These practices include procedures for the sampling of
bility of regulatory limitations prior to use.
thevariousferroalloysandsteeladditives,eitherbeforeorafter
shipment from the plants of the manufacturers. They are
2. Referenced Documents
designed to give results representative of each lot that will be
comparable with the manufacturer’s guaranteed analysis for
2.1 ASTM Standards:
the same lot. For check analysis, the purchaser may use any E11 Specification for Woven Wire Test Sieve Cloth and Test
sampling procedure he desires, but the analytical results
Sieves
obtained on such samples shall not be a basis for complaint or E354 Test Methods for Chemical Analysis of High-
rejection, unless the procedure followed is of an accuracy
Temperature,Electrical,Magnetic,andOtherSimilarIron,
equivalent to that prescribed in these methods. Nickel, and Cobalt Alloys
E135 Terminology Relating to Analytical Chemistry for
1.2 In sampling ferroalloys and steel additives, serious
Metals, Ores, and Related Materials
errors often occur from contamination of the samples by iron
from the sampling appliances. Therefore, special precautions
3. Terminology
should be observed to avoid this source of error. Metallic iron
may be removed with a magnet from nonmagnetic alloys; its
3.1 Definitions—Except as defined as follows, for defini-
estimationinotheralloysrequiresspecialanalyticalprocedures tions of terms used in this guide, refer to Terminology E135.
(Note 1). To avoid this error, parts of crushers and pulverizing
equipment contacting the samples shall be of steel or other
4. Significance and Use
material showing a high resistance to abrasion of the type
4.1 Thesepracticesforthesamplingofmetalsandalloysare
involved.
primarily intended to test such materials for compliance with
NOTE 1—Metallic iron in ferrochromium and ferrosilicon may be compositional specifications. It is assumed that all who use
determined as follows: Transfer5gofthe sample of alloy to a 150-mL
these methods will be trained samplers capable of performing
beaker,add25mLofHNO (1 + 3),cover,boil5min,filterintoa250-mL
common sampling procedures skillfully and safely.
beaker, and wash with hot water. Add NH OH in slight excess, heat to
boiling, filter, and wash with hot water. Dissolve the precipitate on the
5. Apparatus for Preparing Samples
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
5.1 The following equipment is required for the preparation
in Test Method E354.
of analytical samples of ferroalloys:
1.3 The values stated in SI units are to be regarded as the
5.1.1 Crusher—A strongly built jaw crusher capable of
standard. The inch-pound values in parenthesis are given for
rapidly crushing 100-mm (4-in.) lumps to sizes 6.4 mm ( ⁄4 in.)
information only.
and smaller shall be used. The crushing plates of this machine
1.4 This standard does not purport to address all of the
shall be made of a hard and abrasion-resistant steel, such as
safety concerns, if any, associated with its use. It is the manganesesteeloraproperlyhardenedalloyorhypereutectoid
carbon steel.
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 Nov. 27, 2006. Published November 2006. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1939. Last previous edition approved in 2001 as E32 – 86 (2001). DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E0032-86R06E01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E32 − 86 (2006)
5.1.2 Roll Crusher—A roll crusher, the rolls of which are material and conditions, such as each cast, each carload, each
fitted with tires of hardened and tempered chromium steel to ladleful, or each binful.
avoid iron contamination of the sample, shall be used to reduce
6.2 Division of Samples—In these methods the term “di-
the 6.4-mm ( ⁄4-in.) pieces to a particle size that will pass the
vide” is used to indicate a division of a sample into two
No. 10 (2.00-mm) sieve and be retained on the No. 20
approximately equal parts of similar composition as in riffling.
(850-µm) sieve.
5.1.3 Riffles—Riffles, also designated as Jones dividers, are
7. Sampling Spiegeleisen and 15 % Ferrosilicon
usually preferable to the use of hand methods for dividing
7.1 Spiegeleisen is generally cast in pigs and shipped in
samples. Riffles with openings of 12.7, 25.4, 50.8, and 76.2
bulk. Since this alloy is very hard and somewhat tough,
1 1
mm ( ⁄2, 1, 2, and 3 in.) should be available; the ⁄2-in. riffle to
sampling is most accurately and easily accomplished during
be used for samples containing particles up to 3.2 mm ( ⁄8 in.)
the tapping of the metal from the furnace or during the
in size, the 1-in. riffle for samples containing particles up to 9.6
pig-casting operation by taking small spoonfuls and pouring
mm ( ⁄8 in.), the 2-in. for samples containing particles up to
themetalquicklyintoatestmolddesignedtosolidifythemetal
19.1 mm ( ⁄4 in.), and the 3-in. for samples containing particles
quicklyandgiveacleantestpigthatiseasilybroken.Sampling
up to 50.8 mm (2 in.) in size. Riffles should be of the enclosed
ofthemetalinthesolidstateisdifficult,andisbestdoneduring
type to reduce dust losses. The use of multiple riffles is not
the loading or unloading, except when the material is loaded
approved.
from bins or unloaded by dumping. The procedure, therefore,
5.1.4 Mortar and Pestle—The mortar and pestle shall both
may be varied to suit the conditions but shall always conform
be made of properly hardened alloy steel of a kind and grade
to the following requirements:
designed to resist severe abrasive forces (Note 2). Suitable
7.1.1 Sampling at Furnace—The purchaser may arrange
dimensions of the mortar are 79.4 mm (3 ⁄8 in.) in outside
with the manufacturer to have the sampling done at the
height, 76.2 mm (3 in.) in outside diameter, 39.7 mm (1 ⁄16 in.)
furnace. If so, each shipment or each cast may constitute a unit
in inside diameter, and 60.3 mm (2 ⁄8 in.) in inside depth, the
sample for analyzing. The sample shall be obtained by collect-
bottom 12.7 mm ( ⁄2 in.) of which shall be rounded. The pestle
ing portions with a spoon from the runner as the metal flows
shall be 152 mm (6 in.) in length, 38.1 mm (1 ⁄2 in.) in
from the furnace, unless the metal is treated in the runner or
diameter, and rounded at the bottom. The upper part of the
ladle to change its composition, in which event the portions
pestle should be slightly softer than the remainder in order to
shall be taken as the metal flows from the ladle to the pig
decrease the tendency to shatter. Both the mortar and pestle,
casting machine. In any case, at least two spoonfuls of metal
after hardening, shall be polished with abrasive paper to
shall be taken from each ladle, one spoonful while the first
remove all scale. The narrow clearance between the pestle and
third of a ladleful is flowing into or from the ladle and the
the sides of the mortar reduces the dust loss.
second while the last third is flowing. Each spoonful shall be
taken in a manner to avoid collecting dirt or slag, and the clean
NOTE 2—For example: steel mortars and pestles of the following
metalshallbeimmediatelypouredintoacleanshallowmoldto
composition, after proper hardening and tempering treatments, have been
found satisfactory:
form a thin chill casting from which small pieces approxi-
Carbon, % 0.60 mately equal in size may be readily broken. When the
Manganese, % 0.25
spiegeleisen is cast in sand beds, the molten metal being run
Phosphorus, % 0.02
from the furnace directly to the casting floor, the samples shall
Sulfur, % 0.02
Silicon, % 0.25
be taken by dipping skimmed molten metal from the runner
Chromium, % 1.25
trough and pouring it into a small quartered cast-iron button
Tungsten, % 2.20
mold. A sample shall be taken in this manner to represent the
Vanadium, % 0.10
metal being cast in each pig bed. From the test castings thus
After machining annealed steel of this grade to the usual form and
obtained to represent a shipment, approximately equal portions
dimensions, each part is heated to between 760 and 800°C, quenched in a
shall be taken and combined to form the sample which shall
light, mineral quenching oil and tempered at once. The pestle may be
have a gross mass of not less than 200 g.The sample shall then
treated by quenching the lower portion only, the upper portion being
be alternately crushed in a mortar and sieved until it all passes
permitted to air cool, and then tempering the quenched portion.
through a No. 80 (180-µm) sieve. If the sample is to be
NOTE 3—Mechanically operated pulverizing equipment such as a ring
pulverizer may be substituted for the mortar and pestle, provided suitable
analyzed by more than one laboratory, it shall be mixed, coned,
tests show that the use of such equipment does not affect the composition
and quartered upon glazed paper (Note 4). The sample or
of a sample of any material obtained by these methods.
samples thus prepared shall be thoroughly mixed, dried for 1 h
5.1.5 Sieves—The sieves shall conform to Specification
at 105 to 110°C, and preserved for analysis in well-stoppered
E11.
bottles properly labeled for full identification, including the
name of the material, the manufacturer, the date, the cast or lot
6. Unit Quantities for Sampling and Analysis
number, etc.
6.1 Each shipment, except as otherwise agreed upon by the
NOTE 4—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 Sampling Solid Forms—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
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E32 − 86 (2006)
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
fixedplanwhichassurestheobtainingofpiecescomprisingthe 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 No. 10
mately in half by any convenient means, and one of the halves
(2.00-mm)sieve.A170-to220-g6-to8-ozportionobtainedby
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 No. 100 (150-µm) 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 sample shall
contains portions of the outer surface which may be contami-
bepoureduponglazedpaper,mixedthoroughly,anddivided,if
nated with sand or other foreign material. The spallings from
necessary (Note 4) by quartering, dried for1hat105to110°C,
each half pig as collected shall be placed in separate envelopes
and then preserved in a well-stoppered bottle or bottles.
and weighed to the nearest 1 g. Each portion so selected shall
8.3 Crushed Alloy (below 50.8 mm (2 in.) in size)—One
be of approximately the same mass.
container out of every five in the shipment shall be opened and
7.1.2.1 The portions shall then be combined to form the
the contents dumped. A sample representative of both lumps
sample and alternately crushed (preferably in a hardened-alloy
and fines shall be taken from each of the dumped containers to
steel mortar) and sieved until it passes a No. 6 (3.35-mm)
give a combined sample of approximately 0.5 % of the mass of
sieve. Between 280 and 420 g (10 and 15 oz) shall then be
the lot or shipment, this sample being composed of equal
separated from the crushed sample by riffling and this portion
amounts of the samples taken from all containers dumped. If in
shall be pulverized to pass a No. 80 (180-µm) sieve. The
bulk, a fixed portion of representative material shall be taken
pulverizing of over-sizes is best done with the hardened
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