ASTM E1306-22

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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: E1306 − 17 E1306 − 22
Standard Practice for
Preparation of Metal and Alloy Samples for Chemical
Analysis by Electric Arc RemeltingMelting for
Spectrochemical Analysis
This standard is issued under the fixed designation E1306; 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 This practice covers the preparation of solid samples of reactive and refractory metals and alloys by electric arc remelting. The
samples for melting may be in the form of drillings, chunks, chips, turnings, wires, sponge wire, sponge, powder briquettes, and
powdered metals.
1.1.1 This practice is also suitable for preparation of solid samples of other metals, such as cast irons, steels, stainless steels, tool
steels, nickel, nickel alloys, cobalt, and cobalt alloys.
1.2 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.
1.3 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. Specific hazard statements are given in Section 9.
1.4 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:
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E876 Practice for Use of Statistics in the Evaluation of Spectrometric Data (Withdrawn 2003)
E1010 Practice for Preparation of Disk Specimens of Steel and Iron by Remelting for Spectrochemical Analysis (Withdrawn
2022)
3. Terminology
3.1 Definitions—For definitions of terms used in this practice, refer to Terminology E135.
This practice is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.20 on Fundamental Practices.
Current edition approved May 15, 2017June 15, 2022. Published June 2017July 2022. Originally approved in 1989. Last previous edition approved in 20112017 as
E1306 – 11.E1306 – 17. DOI: 10.1520/E1306-17.10.1520/E1306-22.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1306 − 22
4. Summary of Practice
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4.1 Various forms are melted into a button approximately 132 mm ⁄4 inches(1.25 in.) in diameter and approximately ⁄4
inches6 mm (0.25 in.) thick using an electric arc furnace. The action of the arc creates agitation and mixing of the molten metal
which produces a homogeneous sample.
5. Significance and Use
5.1 This sampling practice is useful for converting material taken from ingots or other solid materials into a homogeneous solid
sample suitable for direct excitation on a spark atomic emission or X-ray fluorescence spectrometer. The resultant button may itself
be chipped to provide specimens for test methods requiring solutions or chips.
5.2 This practice has been used extensively for the preparation of zirconium, zirconium alloy, titanium, and titanium alloy
materials, and is applicable to other reactive, refractory, ferrous and nonferrous alloys, such as cobalt, cobalt alloys, niobium,
nickel, nickel alloys, cast irons, steels, stainless steels, tantalum, tool steels, and tungsten.
6. Interferences
6.1 The user should carefully consider the impact of using remeltedmelted samples for analysis as remelted samples these may
be subject to selective volatilization or segregation of anyvarious elements. Elements known to volatilize are bismuth, cadmium,
chlorine, lead, magnesium, sodium, tellurium, thallium, uranium, and zinc. Other elements that may change in content are the
interstitial gases, oxygen, nitrogen, and hydrogen, plus carbon, which may be added hydrogen. Carbon content may increase if a
graphite anode is used. A tungsten anode may be substituted if carbon pickupcontamination is a concern. Tungsten contamination
may occur if this electrode is used. Copper contamination also concern; however, tungsten contamination may occur. Copper
contamination may be introduced from the melting crucible.
7. Apparatus
7.1 Electric Arc Remit Furnace—Melting Furnace —This section describes the various components of an electric arc
remeltmelting furnace. Refer to Fig. 1 to see how each component is arranged. for component arrangement. The number assigned
Legend:
(1) Anode Housing (7) Jack
(2) Rubber Boot (8) DC Electrical Welder
(3) Relief Valve (9) Pressure Regulator
(4) Inlet Fittings for Argon (10) Vacuum Pump
(5) Outlet Fitting for Vacuum (11) Control Panel
(6) Crucible Housing (12) Power Cable
FIG. 1 Schematic of Electric Arc RemeltMelting Furnace
Melting furnaces, manufactured by Cianflone Scientific, 135 Industry Drive, Pittsburgh, PA 15275, www.cianflone.com, have been found suitable for this purpose.
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to each component in the7.1.1 following descriptionthrough 7.8 corresponds to the number in Fig. 1the schematic. A safety
interlock shall be provided to prevent electrical shock when the melting furnace is open.
7.1.1 Water-Cooled Upper Housing (1), (1), approximately 6 inches152 mm (6 in.) in diameter and 6159 mm ⁄4 inches(6.25 in.)
in height, and having a smooth, flat sealing surface.
7.1.1.1 This upper housing may be equipped with a viewing window composed of dark welding-type glass with an inner protective
glass that is impervious to heat and splatter from the molten sample.
7.1.2 Rubber Boot—(2), shall cover the anode manipulator assembly to prevent electrical shock.
7.1.2.1 The anode manipulator assembly (or electrode holder) can typically be moved up and down and in a circular motion to
facilitate spacing between the anode and the sample to enable the arc to effectively melt the sample. See 12.5.
7.1.3 The top of the housing shall be fabricated from an electrical and thermal insulating material, such as Bakelite, and shall
support the following items:
7.1.3.1 Relief Valve—(3), to relieve excessive pressure during the melting process.
7.1.3.2 Inlet Fitting—(4), for argon.
7.1.3.3 Outlet Fitting—(5), for connecting to a vacuum pump.
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7.1.4 Water-Cooled Lower Housing (6), (6), approximately 5146 mm ⁄4 inches(5.75 in.) in diameter and 5140 mm ⁄2
inches(5.5 in.) in height containing the copper melting crucible. Its upper surface shall be fitted with a neoprene O-ring to seal
against the upper anode housing.
7.1.4.1 The lower housing shall be capable of being inverted for removal of the button after it has cooled.
7.1.5 Jack—(7), to raise the lower housing against the upper anode housing, compressing the O-ring and sealing the crucible
chamber.
7.2 DC Electric Welder—(8), to provide an arc current of 400 A to 800 A.
7.3 Pressure Regulator—(9), two-stage, for argon gas.
7.4 Vacuum Pump—(10), having an initial pumping rate of 5050 L L/min ⁄min or more.
7.5 Wire Brushes, to clean the crucible.
7.6 Tamping Rod, suitable for packing the sample into the crucible.
7.7 Foot Switch, Optional, to provide low and high power settings (optional). settings. If a foot switch is not available,provided,
the low to high power and the high to low power transition can be performed with thea rheostat designed for adjusting the current.
7.8 Control Panel (11), (11), containing the master power switch and rheostat for adjusting the current.
8. Reagents and Materials
8.1 Argon Gas, 99.99 %, 99.99 % purity, supplied from a gas or liquid tank.
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8.2 Anode, graphite or tungsten, ⁄2 inches approximately 13 mm (0.5 in.) in diameter and 264 mm ⁄2 inches(2.5 in.) in length with
a tapered tip.
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9. Hazards
9.1 Wear safety glasses with side shields, or full face shield.
9.2 Wear insulated gloves when changing hot electrodes and handling hot buttons.
9.3 An electrical shock hazard exists if the rubber boot is removed from around the anode manipulator assembly at the top of the
furnace.
9.4 If fumes evolved off during melting have been are determined to be hazardous, then an exhaust vent should be installed over
the furnace.
9.5 Follow the manufacturer’s instructions to avoid electrical shock and harm from light and heat.
10. Sample Preparation
10.1 Remove any organic contamination and dry thoroughly before melting. Compacting fine powders, chips, drillings, turnings,
or wire into a briquette may provide more consistent melting.
11. Preparation of Apparatus
11.1 Initial Setup—Refer to Fig. 1.
11.1.1 Attach the cooling water to the apparatus and adjust the flow rate per manufacturer’s recommendations.instructions.
11.1.2 Attach the argon supply and adjust the two-stage regulator output per manufacturer’s recommendations.instructions.
11.1.3 Attach the vacuum pump.
11.1.4 Attach the dc electric welder to the apparatus at the control panel.
11.1.5 Attach the graphite anode to the manipulator assembly.
11.2 Preparation of Anode—The lifetime of the anode can be extended significantly by dipping it into the molten metal. When
this procedure is used, it is imperative that there be a separate anode for each type of metal or alloy to prevent cross contamination
of the samples.
12. Procedure
12.1 Turn on the water valve and the master power switch. Adjust the current at the control box so that the low power setting will
be 400 A and the high power setting will be 800 A. 800 A. A fixed power between 400 A and 800 A 400 A and 800 A can also
be used.
Caution—When melting fine powders, use an initial current of 100 A until the powder appears to be well fused. Raise the
current to 300 A and complete the melting. This will help prevent loss of sample due to splattering of the powder when the arc
is first struck.
12.2 Clean the melting crucible with a wire brush before each melt.
12.3 Charging the Crucible:
12.3.1 Weigh sufficient sample to fill the crucible. Material density and the form and size of th
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