ASTM E32-86(2001)
(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
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 1). 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 Methods E38.
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:E32–86 (Reapproved 2001)
Standard Practices for
Sampling Ferroalloys and Steel Additives for Determination
of Chemical Composition
ThisstandardisissuedunderthefixeddesignationE 32;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 These practices include procedures for the sampling of
thevariousferroalloysandsteeladditives,eitherbeforeorafter E 11 Specification for Wire-Cloth Sieves for Testing Pur-
shipment from the plants of the manufacturers. They are poses
designed to give results representative of each lot that will be E 38 Methods for Chemical Analysis of Nickel-Chromium
comparable with the manufacturer’s guaranteed analysis for and Nickel-Chromium-Iron Alloys
the same lot. For check analysis, the purchaser may use any
3. Significance and Use
sampling procedure he desires, but the analytical results
3.1 Thesepracticesforthesamplingofmetalsandalloysare
obtained on such samples shall not be a basis for complaint or
rejection, unless the procedure followed is of an accuracy primarily intended to test such materials for compliance with
compositional specifications. It is assumed that all who use
equivalent to that prescribed in these methods.
1.2 In sampling ferroalloys and steel additives, serious these methods will be trained samplers capable of performing
common sampling procedures skillfully and safely.
errors often occur from contamination of the samples by iron
from the sampling appliances. Therefore, special precautions
4. Apparatus for Preparing Samples
should be observed to avoid this source of error. Metallic iron
4.1 The following equipment is required for the preparation
may be removed with a magnet from nonmagnetic alloys; its
of analytical samples of ferroalloys:
estimationinotheralloysrequiresspecialanalyticalprocedures
4.1.1 Crusher—A strongly built jaw crusher capable of
(Note 1). To avoid this error, parts of crushers and pulverizing
rapidly crushing 100-mm (4-in.) lumps to sizes 6.4 mm ( ⁄4 in.)
equipment contacting the samples shall be of steel or other
and smaller shall be used. The crushing plates of this machine
material showing a high resistance to abrasion of the type
shall be made of a hard and abrasion-resistant steel, such as
involved.
manganesesteeloraproperlyhardenedalloyorhypereutectoid
NOTE 1—Metallic iron in ferrochromium and ferrosilicon may be
carbon steel.
determined as follows: Transfer5gofthe sample of alloy to a 150-mL
4.1.2 Roll Crusher—A roll crusher, the rolls of which are
beaker,add25mLofHNO (1 + 3),cover,boil5min,filterintoa250-mL
fitted with tires of hardened and tempered chromium steel to
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 avoid iron contamination of the sample, shall be used to reduce
paper with a minimum quantity of hot HCl (1 + 2), wash the filter with hot
the 6.4-mm ( ⁄4-in.) pieces to a particle size that will pass the
water, and titrate the iron by a standard procedure such as that described
No. 10 (2.00-mm) sieve and be retained on the No. 20
in Methods E 38.
(850-µm) sieve.
1.3 The values stated in SI units are to be regarded as the
4.1.3 Riffles—Riffles, also designated as Jones dividers, are
standard. The inch-pound values in parenthesis are given for
usually preferable to the use of hand methods for dividing
information only.
samples. Riffles with openings of 12.7, 25.4, 50.8, and 76.2
1 1
1.4 This standard does not purport to address all of the
mm ( ⁄2, 1, 2, and 3 in.) should be available; the ⁄2-in. riffle to
safety concerns, if any, associated with its use. It is the
be used for samples containing particles up to 3.2 mm ( ⁄8 in.)
responsibility of the user of this standard to establish appro-
in size, the 1-in. riffle for samples containing particles up to 9.6
priate safety and health practices and determine the applica-
mm ( ⁄8 in.), the 2-in. for samples containing particles up to
bility of regulatory limitations prior to use.
19.1 mm ( ⁄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
1 approved.
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 April 25, 1986. Published August 1986. Originally Annual Book of ASTM Standards, Vol 14.02.
published as E 32 – 39 T replacing former A 103. Last previous edition E 32 – 86. Discontinued; see 1989 Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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4.1.4 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
6.1.1 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
metalshallbeimmediatelypouredintoacleanshallow mold to
composition, after proper hardening and tempering treatments, have been
form a thin chill casting from which small pieces approxi-
found satisfactory:
mately equal in size may be readily broken. When the
Carbon, % 0.60
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
be taken by dipping skimmed molten metal from the runner
Silicon, % 0.25
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
at 105 to 110°C, and preserved for analysis in well-stoppered
4.1.5 Sieves—The sieves shall conform to Specification
bottles properly labeled for full identification, including the
E11.
name of the material, the manufacturer, the date, the cast or lot
number, etc.
5. Unit Quantities for Sampling and Analysis
5.1 Each shipment, except as otherwise agreed upon by the
NOTE 4—Finished samples are frequently divided into four portions:
purchaser and the manufacturer, shall constitute a unit for one for the purchaser, one for the manufacturer, one for an umpire if
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
6.1.2 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
material and conditions, such as each cast, each carload, each
random pigs or pieces at regular intervals during the loading or
ladleful, or each binful.
unloading. Surface sampling of piles of the material will not
5.2 Division of Samples—In these methods the term “di-
give a representative sample. When piles of the material must
vide” is used to indicate a division of a sample into two
be sampled, the pieces shall be selected according to some
approximately equal parts of similar composition as in riffling.
fixed plan which assures the obtaining of pieces comprising the
gross sample from uniformly distributed points throughout, a
6. Sampling Spiegeleisen and 15 % Ferrosilicon
condition requiring the moving of all or many of the pieces in
6.1 Spiegeleisen is generally cast in pigs and shipped in the pile. For lots of 45 Mg (50 tons) or larger, 1 pig or piece
bulk. Since this alloy is very hard and somewhat tough, shall be taken for each 9 Mg (10 tons), and for small lots the
sampling is most accurately and easily accomplished during number of pieces shall be proportionately increased to 10
the tapping of the metal from the furnace or during the pieces for a 9-Mg (10-ton) lot, or 5 pieces for a 0.9-Mg (1-ton)
pig-casting operation by taking small spoonfuls and pouring lot. The various pigs thus collected shall be broken approxi-
themetalquicklyintoatestmolddesignedtosolidifythemetal mately in half by any convenient means, and one of the halves
quicklyandgiveacleantestpigthatiseasilybroken.Sampling of each pig shall be reserved. From the fractured surface of
ofthemetalinthesolidstateisdifficult,andisbestdoneduring each of these half pigs, an approximately equal portion shall be
the loading or unloading, except when the material is loaded taken by any suitable means (as by spalling with a heavy
from bins or unloaded by dumping. The procedure, therefore, hammer), care being taken by the sampler to see that these
E32
spalls are not all from the outer edges of the pigs but at least 150 µm and prevent loss of dust. The pulverized sample shall
some are obtained from the central portion, and that none bepoureduponglazedpaper,mixedthoroughly,anddivided,if
contains portions of the outer surface which may be contami-
necessary (Note 4) by quartering, dried for1hat105to110°C,
nated with sand or other foreign material. The spallings from
and then preserved in a well-stoppered bottle or bottles.
each half pig as collected shall be placed in separate envelopes
7.3 Crushed Alloy (below 50.8 mm (2 in.) in size)—One
and weighed to the nearest 1 g. Each portion so selected shall
container out of every five in the shipment shall be opened and
be of approximately the same mass.
the contents dumped. A sample representative of both lumps
6.1.2.1 The portions shall then be combined to form the
and fines shall be taken from each of the dumped containers to
sample and alternately crushed (preferably in a hardened-alloy
give a combined sample of approximately 0.5 % of the mass of
steel mortar) and sieved until it passes a No. 6 (3.35-mm)
the lot or shipment, this sample being composed of equal
sieve. Between 280 and 420 g (10 and 15 oz) shall then be
amounts of the samples taken from all containers dumped. If in
separated from the crushed sample by riffling and this portion
bulk, a fixed portion of representative material shall be taken
shall be pulverized to pass a No. 80 (180-µm) sieve. The
withashovelorscoopatregularintervalsduringtheloadingor
pulverizing of over-sizes is best done with the hardened steel
unloading to accumulate a sample of about 0.5 % of the mass
mortar and pestle, while sieving frequently to keep the size
of the lot.
close to 180-µm and prevent loss of dust. The pulverized
sample shall be thoroughly mixed upon glazed paper, divided
7.3.1 The 0.5 % sample shall be crushed to pass a 25.4-mm
if necessary, labeled, and dried prior to analysis, in accordance
(1-in.)sieve,mixed,anddividedtwiceifitsmassisbetween90
with 6.1.1.
and 135 kg (200 and 300 lb) or three times if it weighs more
than 135 kg (300 lb). The portion reserved shall be crushed to
7. Sampling Ferrosilicon, Standard Ferromanganese,
pass a 6.4-mm ( ⁄4-in.) sieve. Preparation of the sample shall
Silicomanganese, Ferrophosphorus, and 12 to 15 %
then be completed as described for 6.4-mm ( ⁄4-in.) material in
Zirconium Alloy
7.2.
7.1 Alloys in this group are shipped in both lump and
crushed form, in bulk as well as in containers. Carload lots are
8. Sampling High-Carbon Ferrochromium, Medium-
generally shipped in bulk, except the finely crushed sizes
Carbon Ferromanganese, Low-Carbon
which are usually shipped in containers. Different procedures
Ferromanganese, Silicon Metal, Calcium-Silicon, and
are required for sampling the lump and the crushed alloy, and
35 to 40 % Zirconium Alloy
the work of sampling is most conveniently done while loading
or unloading.
8.1 These alloys are shipped in both lump and crush form,
7.2 Lump Alloy (above 50.8 mm (2 in.) in size)—In sam-
bulk, or in containers.
pling bulk shipments, lumps
...
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