ASTM E32-86(1996)e1
(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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e1
Designation: E 32 – 86 (Reapproved 1996)
Standard Practices for
Sampling Ferroalloys and Steel Additives for Determination
of Chemical Composition
This standard is issued under the fixed designation E 32; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Keywords were added in June 1996.
1. Scope bility of regulatory limitations prior to use.
1.1 These practices include procedures for the sampling of
2. Referenced Documents
the various ferroalloys and steel additives, either before or after
2.1 ASTM Standards:
shipment from the plants of the manufacturers. They are
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
designed to give results representative of each lot that will be
poses
comparable with the manufacturer’s guaranteed analysis for
E 38 Methods for Chemical Analysis of Nickel-Chromium
the same lot. For check analysis, the purchaser may use any
and Nickel-Chromium-Iron Alloys
sampling procedure he desires, but the analytical results
obtained on such samples shall not be a basis for complaint or
3. Significance and Use
rejection, unless the procedure followed is of an accuracy
3.1 These practices for the sampling of metals and alloys are
equivalent to that prescribed in these methods.
primarily intended to test such materials for compliance with
1.2 In sampling ferroalloys and steel additives, serious
compositional specifications. It is assumed that all who use
errors often occur from contamination of the samples by iron
these methods will be trained samplers capable of performing
from the sampling appliances. Therefore, special precautions
common sampling procedures skillfully and safely.
should be observed to avoid this source of error. Metallic iron
may be removed with a magnet from nonmagnetic alloys; its
4. Apparatus for Preparing Samples
estimation in other alloys requires special analytical procedures
4.1 The following equipment is required for the preparation
(Note 1). To avoid this error, parts of crushers and pulverizing
of analytical samples of ferroalloys:
equipment contacting the samples shall be of steel or other
4.1.1 Crusher—A strongly built jaw crusher capable of
material showing a high resistance to abrasion of the type
rapidly crushing 100-mm (4-in.) lumps to sizes 6.4 mm ( ⁄4 in.)
involved.
and smaller shall be used. The crushing plates of this machine
NOTE 1—Metallic iron in ferrochromium and ferrosilicon may be
shall be made of a hard and abrasion-resistant steel, such as
determined as follows: Transfer5gofthe sample of alloy to a 150-mL
manganese steel or a properly hardened alloy or hypereutectoid
beaker, add 25 mL of HNO (1 + 3), cover, boil 5 min, filter into a 250-mL
carbon steel.
beaker, and wash with hot water. Add NH OH in slight excess, heat to
4.1.2 Roll Crusher—A roll crusher, the rolls of which are
boiling, filter, and wash with hot water. Dissolve the precipitate on the
fitted with tires of hardened and tempered chromium steel to
paper with a minimum quantity of hot HCl (1 + 2), wash the filter with hot
avoid iron contamination of the sample, shall be used to reduce
water, and titrate the iron by a standard procedure such as that described
in Methods E 38.
the 6.4-mm ( ⁄4-in.) pieces to a particle size that will pass the
No. 10 (2.00-mm) sieve and be retained on the No. 20
1.3 The values stated in SI units are to be regarded as the
(850-μm) sieve.
standard. The inch-pound values in parenthesis are given for
4.1.3 Riffles—Riffles, also designated as Jones dividers, are
information only.
usually preferable to the use of hand methods for dividing
1.4 This standard does not purport to address all of the
samples. Riffles with openings of 12.7, 25.4, 50.8, and 76.2
safety problems, if any, associated with its use. It is the
1 1
mm ( ⁄2, 1, 2, and 3 in.) should be available; the ⁄2-in. riffle to
responsibility of the user of this standard to establish appro-
be used for samples containing particles up to 3.2 mm ( ⁄8 in.)
priate safety and health practices and determine the applica-
in size, the 1-in. riffle for samples containing particles up to 9.6
mm ( ⁄8 in.), the 2-in. for samples containing particles up to
19.1 mm ( ⁄4 in.), and the 3-in. for samples containing particles
These practices are under the jurisdiction of ASTM Committee E-1 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, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E32
up to 50.8 mm (2 in.) in size. Riffles should be of the enclosed the loading or unloading, except when the material is loaded
type to reduce dust losses. The use of multiple riffles is not from bins or unloaded by dumping. The procedure, therefore,
approved. may be varied to suit the conditions but shall always conform
4.1.4 Mortar and Pestle—The mortar and pestle shall both to the following requirements:
be made of properly hardened alloy steel of a kind and grade
6.1.1 Sampling at Furnace—The purchaser may arrange
designed to resist severe abrasive forces (Note 2). Suitable
with the manufacturer to have the sampling done at the
dimensions of the mortar are 79.4 mm (3 ⁄8 in.) in outside
furnace. If so, each shipment or each cast may constitute a unit
height, 76.2 mm (3 in.) in outside diameter, 39.7 mm (1 ⁄16 in.)
sample for analyzing. The sample shall be obtained by collect-
in inside diameter, and 60.3 mm (2 ⁄8 in.) in inside depth, the
ing portions with a spoon from the runner as the metal flows
bottom 12.7 mm ( ⁄2 in.) of which shall be rounded. The pestle
from the furnace, unless the metal is treated in the runner or
shall be 152 mm (6 in.) in length, 38.1 mm (1 ⁄2 in.) in
ladle to change its composition, in which event the portions
diameter, and rounded at the bottom. The upper part of the
shall be taken as the metal flows from the ladle to the pig
pestle should be slightly softer than the remainder in order to
casting machine. In any case, at least two spoonfuls of metal
decrease the tendency to shatter. Both the mortar and pestle,
shall be taken from each ladle, one spoonful while the first
after hardening, shall be polished with abrasive paper to
third of a ladleful is flowing into or from the ladle and the
remove all scale. The narrow clearance between the pestle and
second while the last third is flowing. Each spoonful shall be
the sides of the mortar reduces the dust loss.
taken in a manner to avoid collecting dirt or slag, and the clean
metal shall be immediately poured into a clean shallow mold to
NOTE 2—For example: steel mortars and pestles of the following
form a thin chill casting from which small pieces approxi-
composition, after proper hardening and tempering treatments, have been
found satisfactory: mately equal in size may be readily broken. When the
spiegeleisen is cast in sand beds, the molten metal being run
Carbon, % 0.60
Manganese, % 0.25
from the furnace directly to the casting floor, the samples shall
Phosphorus, % 0.02
be taken by dipping skimmed molten metal from the runner
Sulfur, % 0.02
trough and pouring it into a small quartered cast-iron button
Silicon, % 0.25
Chromium, % 1.25
mold. A sample shall be taken in this manner to represent the
Tungsten, % 2.20
metal being cast in each pig bed. From the test castings thus
Vanadium, % 0.10
obtained to represent a shipment, approximately equal portions
After machining annealed steel of this grade to the usual form and
shall be taken and combined to form the sample which shall
dimensions, each part is heated to between 760 and 800°C, quenched in a
have a gross mass of not less than 200 g. The sample shall then
light, mineral quenching oil and tempered at once. The pestle may be
be alternately crushed in a mortar and sieved until it all passes
treated by quenching the lower portion only, the upper portion being
through a No. 80 (180-μm) sieve. If the sample is to be
permitted to air cool, and then tempering the quenched portion.
NOTE 3—Mechanically operated pulverizing equipment such as a ring analyzed by more than one laboratory, it shall be mixed, coned,
pulverizer may be substituted for the mortar and pestle, provided suitable
and quartered upon glazed paper (Note 4). The sample or
tests show that the use of such equipment does not affect the composition
samples thus prepared shall be thoroughly mixed, dried for 1 h
of a sample of any material obtained by these methods.
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
NOTE 4—Finished samples are frequently divided into four portions:
5.1 Each shipment, except as otherwise agreed upon by the
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
6.1.2 Sampling Solid Forms—When the metal is in the solid
any alloy exceeding 450 Mg (500 tons) be divided into smaller
state, a gross sample shall first be collected by selecting
lots for sampling according to some plan best adapted to the
material and conditions, such as each cast, each carload, each random pigs or pieces at regular intervals during the loading or
unloading. Surface sampling of piles of the material will not
ladleful, or each binful.
give a representative sample. When piles of the material must
5.2 Division of Samples—In these methods the term “di-
be sampled, the pieces shall be selected according to some
vide” is used to indicate a division of a sample into two
fixed plan which assures the obtaining of pieces comprising the
approximately equal parts of similar composition as in riffling.
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-
the metal quickly into a test mold designed to solidify the metal mately in half by any convenient means, and one of the halves
quickly and give a clean test pig that is easily broken. Sampling of each pig shall be reserved. From the fractured surface of
of the metal in the solid state is difficult, and is best done during each of these half pigs, an approximately equal portion shall be
E32
taken by any suitable means (as by spalling with a heavy with the hardened alloy-steel mortar and pestle, or a ring
hammer), care being taken by the sampler to see that these pulverizer, while sieving frequently to keep the size close to
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 be poured upon glazed paper, mixed thoroughly, and divided, 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 with a shovel or scoop at regular intervals during the loading or
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 7.3.1 The 0.5 % sample shall be crushed to pass a 25.4-mm
sample shall be thoroughly mixed upon glazed paper, divided (1-in.) sieve, mixed, and divided twice if its mass is between 90
if necessary, labeled, and dried prior to analysis, in accordance and 135 kg (200 and 300 lb) or three times if it weighs more
with 6.1.1. than 135 kg (300 lb). The portion reserved shall be crushed to
pass a 6.4-mm ( ⁄4-in.) sieve. Preparation of the sample shall
7. Sampling Ferrosilicon, Standard Ferromanganese,
then be completed as described for 6.4-mm ( ⁄4-in.) material in
Silicomanganese, Ferrophosphorus, and 12 to 15 %
7.2.
Zirconium Alloy
8. Sampling High-Carbon Ferrochromium, Medium-
7.1 Alloys in this group are shipped in both lump and
Carbon Ferromanganese, Low-Carbon
crushed form, in bulk as well as in containers. Carload lots are
Ferromanganese, Silicon Metal, Calcium-Silicon, and
generally shipped in bulk, except the finely crushed sizes
35 to 40 % Zirconium Alloy
which are usually shipped in containers. Different procedures
are re
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