Designation: E716 − 10

Standard Practices for

Sampling and Sample Preparation of Aluminum and
Aluminum Alloys for Determination of Chemical
Composition by Spectrochemical Analysis1
This standard is issued under the fixed designation E716; 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 E607 Test Method for Atomic Emission Spectrometric

1.1 These practices describe procedures for producing a Analysis Aluminum Alloys by the Point to Plane Tech-
chill cast disk sample from molten aluminum during the nique Nitrogen Atmosphere (Withdrawn 2011)3
production process, and from molten metal produced by E1251 Test Method for Analysis of Aluminum and Alumi-
melting pieces cut from products. num Alloys by Spark Atomic Emission Spectrometry
1.2 These practices describe a procedure for obtaining 3. Terminology
qualitative results by direct analysis of product using spark
atomic emission spectroscopy. 3.1 For definitions of terms used in this practice, refer to
Terminology E135.
1.3 These practices describe procedures for preparation of
samples and products prior to analysis. 4. Summary of Practices
1.4 The values stated in SI units are to be regarded as 4.1 Molten metal representative of the furnace melt is
standard. The values given in parentheses are mathematical poured or drawn by vacuum into a specified mold to produce
conversions to inch-pound units that are provided for informa- a chill-cast disk. The disk is machined to a specified depth that
tion only and are not considered standard. represents the average composition and produces an acceptable
1.5 This standard does not purport to address all of the surface for analysis by spark atomic emission spectroscopy.
safety problems, if any, associated with its use. It is the
4.2 Pieces of solid aluminum fabricated, cast, or wrought
responsibility of the user of this standard to establish appro-
products are remelted and cast into molds or briquetted then
priate safety and health practices and determine the applica-
remelted and cast into molds.
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in 6.1 and 7.2. 4.3 Product can be qualitatively analyzed directly without
remelting after suitable surface preparation. Product with
2. Referenced Documents insufficient mass for direct analysis may be bonded to more
massive material prior to analysis.
2.1 ASTM Standards:2
E135 Terminology Relating to Analytical Chemistry for 4.4 Special practices are included for the sampling and
Metals, Ores, and Related Materials analysis of aluminum-silicon alloys, containing greater than
E401 Practice for Bonding Thin Spectrochemical Samples 14 % silicon.
and Standards to aGreater Mass of Material (Withdrawn
1995)3 5. Significance and Use
5.1 The practice for taking a sample of molten metal during
production and producing a chill cast disk, used in conjunction
1
These practices are under the jurisdiction of ASTM Committee E01 on with the following appropriate quantitative spark atomic emis-
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.04 on Aluminum and Magnesium. sion spectrochemical methods, Test Methods E607 and E1251,
Current edition approved Sept. 1, 2010. Published December 2010. Originally is suitable for use in manufacturing control or certifying, or
approved in 1980. Last previous edition approved in 2002 as E716 – 94 (2002). both, that the entire lot of alloy sampled meets established
DOI: 10.1520/E0716-10.
2
composition limits.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM 5.2 The practice for melting a piece of a product to produce
Standards volume information, refer to the standard’s Document Summary page on
a chill cast disk analyzed in conjunction with the following
the ASTM website.
3
The last approved version of this historical standard is referenced on appropriate quantitative spark atomic emission spectrochemi-
www.astm.org. cal methods, Test Methods E607 and E1251, is suitable, if a

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

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 E716 − 10
representative sample is taken, for determining if the piece throat for the sprue. A slight taper, 1° to 2°, on the hinged
sampled meets Aluminum Association composition limits. portion of the mold facilitates opening when a disk has been
5.3 The practice for direct analysis of product is suitable for cast. The mold material should be steel or cast iron and should
determining an approximate composition of the piece analyzed weigh approximately 3.5 kg to 4.5 kg (8 lb to 10 lb).
6.2.2 Vacuum Mold5is shown in Fig. 2. This mold produces
6. Apparatus disks that are 38 mm (1.5 in.) in diameter and 13 mm (0.5 in.)
thick and weigh approximately 40 g (1.4 oz). The mold con-
6.1 Ladle, capable of holding a minimum of 250 g (8.8 oz)
sists of a solid copper base and a porous bronze wall in the
of molten metal, with a handle of sufficient length to reach into
form of a composite mold insert which is located in a steel
a furnace, trough, or crucible. The ladle should be lightly
mold body. A graphite coated cast iron tip is attached to the
coated with a tightly adhering ladle wash that will serve in part
mold body by a spring clamp assembly. The vacuum source is
to prevent contamination of the sample and also prevent
typically a rubber syringe bulb connected to the mold body.
contact of molten aluminum with metal oxides, that is, rust.
6.2.3 Other Types of Molds—Other molds of different types,
(Warning—Traces of moisture in the coating may cause
materials, and dimensions may be substituted provided that the
dangerous spattering.)
uniformity of the samples so obtained is sufficient for the
NOTE 1—A suitable ladle wash may be prepared as follows: Mix 255 g intended use of the results. Furthermore such samples should
(9 oz) of fine whiting (CaCO3) with 3.8 L (1 gal) of water and boil for have a sizeable area that represents the bulk composition of the
20 min. Add 127 g (4.5 oz) of sodium silicate solution (40 °Bé to 42 °Bé)
and boil for 30 min. Stir well before using.
entire sample and have a spectrochemical response similar to
NOTE 2—Molten aluminum in contact with rust may initiate a thermite the reference materials used for preparing the analytical curve.
reaction. 6.3 Lathe or Milling Machine, capable of machining a
6.2 Sample Molds shall be capable of producing homog- smooth flat surface and capable of repeating the selected depth
enous chill-cast disks having smooth surfaces, free of surface of cut to within 60.013 mm (60.005 in.).
pockets and porosity. These chill cast disks should have a 6.4 Tool Bits—Diamond tipped, alloy steel, or cemented
spectrochemical response similar to the reference materials carbide bits are recommended. The best shape of the lathe tool
used in preparing the analytical curves and should at least have varies with the type and speed of the lathe. A tool bit design
a spark to spark repeatability of no more than 2 % relative on that has been found satisfactory for most aluminum alloys is
major elements. They must be representative of the melt in the shown in Fig. 3.
region excited. Several types of molds have been found
acceptable: 6.5 Portable Electric Melting Furnace,6equipped with a
6.2.1 Type B,4center-pour mold, is shown in Fig. 1. The graphite crucible with a minimum capacity of 200 g (7.1 oz) of
advantage of this mold is that the sample obtained may be molten aluminum and capable of maintaining temperatures for
excited around the entire annular area. This mold produces a melting aluminum alloys.
horizontally cast disk with the sprue over the center of one
side. The mold dimensions are such as to produce a disk 7. Materials
approximately 50 mm to 64 mm (1.97 in. to 2.5 in.) in diameter 7.1 Graphite Rods, of suitable diameter for stirring the
by 6 mm to 13 mm (0.24 in. to 0.50 in.) in thickness. A circular molten aluminum.
central recess 10 mm to 20 mm (0.4 in. to 0.8 in.) in diameter 7.2 Phosphorus, red, amorphous, or other suitable source of
on one side of the disk facilitates machining of that side in phosphorus for grain refining of high silicon alloys during the
preparation for excitation. It also promotes more uniform
freezing of the raised peripheral area, but the corresponding
raised portion of the mold must not be so large as to restrict the 5
A portable Vacuum Sampler, available from Aluminum Company of America,
Alcoa Center, PA 15069, has been found suitable for this purpose.
6
A Jelrus Handy-Melt furnace and graphite crucible, available from Cole-Parmer
4
Instrument Co., 7425 North Oak Park Ave., Chicago, IL 60648, has been found
Type B molds, available from Machine and Welding Incorporated, 713 Fortune
suitable for this purpose.
Crescent, Kingston, ON Canada K7P 2T4, have been found suitable for this purpose.

FIG. 1 Type B Mold

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 E716 − 10
obtaining metal well beneath the surface minimizes the danger
of inclusion of small particles of oxide.
8.1.1.2 Unless the mold is already hot, cast a preliminary
disk into the clean mold in order to preheat it and discard this
disk. Remove excess metal from the ladle, dip into the molten
metal as before, and fill the mold with an even rate of pour
which allows the escape of air from the mold. Do not dump the
metal into the mold. Avoid overfilling the sprue, otherwise the
mold may be difficult to open. Allow the metal to freeze quietly
without jarring. The surface of the disk must be free of any
shrinkage, inclusions, cracks, or roughness.
8.1.2 Chill Cast Disk Using Vacuum Mold—Skim the dross
from the molten metal as in 8.1.1.1, using a skimming tool.
Attach the cast iron mold tip to the mold body using the clamp
arm assembly. Squeez the rubber syringe bulb while immersing
the mold into the metal to prevent oxide skim from entering the
mold tip. Wait about five seconds to allow time for preheating
the sampler. Release the rubber syringe bulb to apply vacuum
that will draw the metal into the sampler. Remove the mold tip
from the metal, detach the mold tip from the mold body, and
FIG. 2 Mold for Vacuum Cast Samples remove the disk. The surface of the disk must be free of any
shrinkage, inclusions, cracks, or roughness.
8.1.3 Machine the disk to appropriate depth for the particu-
lar sampler dimensions. Typically a depth of between 14 % and
22 % of the original thickness corresponds to the composition
on the phase diagram that best represents the average compo-
sition of the whole disk and therefore the actual composition of
the melt. It is advisable to determine the most appropriate
machining depth for the particular disk thickness used and to
target and tightly control that specific depth. Machining to
different depths may result in a different analysis and therefore
cannot be accepted as valid.
NOTE 3—Aluminum samples shall not be prepared by sanding or
grinding. Sanding or grinding tends to smear the relatively soft aluminum
phase over the harder constituent phases or cause hard grains to be torn
from the sample and may cause biased results for spark atomic emission
spectrometry.
FIG. 3 Tool Bit 8.1.3.1 The machined surface must be smooth and free of
scuffs, pits, or inclusions. The ideal surface is neither polished
nor visibly grooved but should be a surface showing very fine
remelt procedure. (Warning—Provide adequate ventilation tool marks. More specifically, the ideal surface may be defined
when phosphorus is added to molten metal.) as approximately a 1.6 × 10−3-mm (63-µin.) standard machine
finish. A surface much finer or much coarser may result in an
8. Preparation of Samples apparent analytical difference. Furthermore, it is important that
8.1 Molten Metal: both sample and reference material have the same machine
8.1.1 Chill-Cast Disk by Molds A or B: finish. Analysis can be made 360° around the disk in the
8.1.1.1 When a furnace or crucible of molten metal is to be annular area adjacent to the edge, avoiding the center area.
sampled, the temperature must be well above the point at 8.1.4 Other Accepted Molds—If molds other than Type B or
which any solid phase could be present. Using the ladle or a the vacuum mold are used, the same instructions given in 8.1
separate skimming tool, coated with a dry, tightly adhering would apply. In addition, since a mold of different dimensions
mold wash (Note 1) and free of any remaining previous metal, may result in a different freezing pattern, each new type of
push as much dross as possible away from the sampling area. mold must be evaluated in order to ascertain the proper depth
Next, dip the ladle sideways into the clear area well below the of machining to represent the true composition of the melt.
surface and stir momentarily. Then turn the ladle upright, and
quickly withdraw. Two things are thus accomplished, namely, 8.2 Remelting and Casting a Sample from Fabricated and
heating the ladle prevents metal freezing on the wall and Cast Products:

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 E716 − 10
8.2.1 Chill-Cast Disk by Type B Mold, or the Vacuum 8.3 Hyper-Eutectic Aluminum-Silicon Alloys (Note 6).
Mold—When the metal to be analyzed is in wrought or cast NOTE 6—These procedures are required only for the accurate determi-
form and a destructive test is applicable, remelt a representa- nation of silicon at levels greater than 14 %. Other elements of interest
tive portion of the metal at a temperature well above the may be determined satisfactorily without either the addition of phosphorus
liquidus line of the alloy. A clay, graphite, or other inert or dilution with high-purity aluminum.
crucible may be used and placed in a convenient laboratory 8.3.1 Analysis Without Dilution:
electric furnace. Then cast a portion of the melt in one of the 8.3.1.1 Molten Metal—Heat the metal to be sampled to
molds as described in 8.1. If the sample is in the form of 760 °C (1400 °F). Preheat the sampling ladle. Add red phos-
turnings, thin sheet, or other finely divided material, remove phorus in a ratio of 1 g (0.036 oz) per 400 g (14.1 oz) of metal
grease or any coatings with a suitable solvent and press into a to a ladle of the melt. Stir briskly with a graphite rod, skim, and
briquet before melting and proceeding as in 8.1. Details of make a preliminary casting, using the special Type B mold
briquet size and formation are not critical to the success of producing a 6-mm (0.24-in.) thick sample. Discard the first
preparing a melt. The largest briquet that can be successfully disk, and make a second disk for analysis. Remove the sprue,
formed and that will fit into the remelt crucible will obviously and machine the sample to a depth of 1.1 mm (0.044 in.) below
speed up the remelt process. Carry out the melting and casting the original surface. Using a carbide-tipped tool which has
operation as rapidly as possible, and use as large melt as been used less than 30 times, continue to machine to a depth of
practical to minimize losses of volatile elements. Follow the 1.2 mm (0.048 in.) below the original surface. A 400-r/min
procedures in 8.1.1-8.1.3 for preheating each particular sam- spindle speed and a 0.68-in. (17-mm) radius/min crossfeed are
pler type. recommended for the final cut. If equivalent analytical perfor-
NOTE 4—Analysis of samples can be used to determine compliance mance can be shown, the use of other materials, such as a
with composition analysis for the piece sampled if a representative sample diamond-tipped bit, may also be used. Reference materials and
is obtained. Direct analysis of samples obtained from fabricated and cast samples shall be machined under identical conditions.
aluminum product shall not be used for determining compliance with 8.3.1.2 Cast Products—When the metal to be analyzed is in
composition specifications. Cast lot composition should be determined cast form, remelt the metal and prepare a disk sample as in
using samples taken during pouring of castings or ingots.
NOTE 5—Remelting is not satisfactory for the determination of volatile 8.3.1.1. Carry out the melting and casting operation as rapidly
elements such as sodium, calcium, lithium, strontium, and some magne- as possible. (See Note 6.)
sium may also be lost if the melt is overheated or kept molten for an 8.3.2 Analysis With Dilution:
excessive time. 8.3.2.1 Molten Metal—Sample the molten metal as in 8.1 or
8.2.2 Direct Analysis of Wrought or Cast Products—Pieces 8.3.1.1, omitting the red phosphorus. Weigh this original
of wrought or cast aluminum product can be analyzed directly sample to 0.01 g, and remelt with a similar amount of 99.99 %
on the surface when the sample preparation procedures de- aluminum in a laboratory electric furnace. Stir thoroughly with
scribed in 8.1 cannot be followed, for example, when there is a graphite rod, and cast a new sample, using any of the molds
insufficient sample for remelting and casting a disk or where described in 6.2. For Type B molds, preheat the mold on a hot
melting would cause loss of a volatile constituent, or where it plate at 177 °C (350 °F) and cast a sample for analysis. Make
is otherwise impractical. The results should be considered vacuum-cast samples by inserting the mold tip into the molten
qualitative and not quantitative. Segregation of elements dur- metal and applying vacuum to draw the metal into the mold
ing solidification and metalurigical differences between the cavity.
product and the reference materials used for calibration may 8.3.2.2 Cast Products—Metal which is in cast form, should
cause biased results. Direct analysis of wrought or cast be remelted and a disk sample prepared as in 8.3.2.1. Complete
aluminum products should not be used to determine compli- the melting and casting operation as rapidly as possible. (See
ance with composition requirements. Note 6.)
8.2.2.1 The sample must be sufficiently massive to prevent 8.3.2.3 Prepare the diluted sample for analysis by removing
undue heating during analysis, and it must have a sufficiently the sprue, and machining Type B disks to a depth of 14 % to
flat surface for excitation. Further, reference materials having a 22 % of the original thickness. It is advisable to determine the
similar spectrochemical response must be available. On sheet most appropriate machining depth for the particular disk
and plate samples, machine-off approximately 0.8 mm thickness used and to target and tightly control that specific
(0.032 in.) or one fourth of the sample thickness, whichever is depth. Machining to different depths may result in a different
the smaller. On other products, machine a flat surface at least analysis and therefore cannot be accepted as valid. Vacuum
1.3 mm (0.052 in.) below the original surface. Choose the cast samples should be machined to a depth of 2.0 mm
depth, location, and number of areas to be analyzed to provide (0.08 in.) below the original surface. Analyze the diluted
a representative analysis of the product. In accordance with sample, using appropriate reference materials with a similar
Practice E401, thin flat material may also be bonded by means composition and metallurgical structure. Dilutions with pure
of a heat and electrically conducting epoxy-type adhesive to a aluminum can be made with ratios other than 1:1 in order to
more massive section to provide a heat sink. In all cases the match the diluted composition with existing reference materi-
prepared area must be large and flat enough to form a good seal als. Volatile elements such as sodium and calcium can be lost
with the spectrometer spark stand table. on remelting and should be determined on the original sample.

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 E716 − 10
9. Calculations for Analysis with Dilution where:
9.1 Calculate the composition of the original sample by W1 = weight of 99.99 % aluminum, and
multiplying the composition of the diluted sample by the W2 = weight of original material to be diluted.
dilution ratio. The dilution ratio is computed as follows:
W 1 1W 2
Dilution ratio 5 (1)
W2

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