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ASTM E1306-94(1998)e1

(Practice)

Standard Practice for Preparation of Metal and Alloy Samples by Electric Arc Remelting for the Determination of Chemical Composition

Standard Practice for Preparation of Metal and Alloy Samples by Electric Arc Remelting for the Determination of Chemical Composition

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 chips, turnings, wires, and sponge. Powdered metals need to be compacted before melting.
1.1.1 This practice is also suitable for preparation of solid samples of other metals, such as steels, stainless steels, tool steels, nickel, nickel alloys, cobalt, and cobalt alloys by electric arc remelting.
1.2 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. Specific hazard statements are given in Section 9.

General Information

Status
Historical
Publication Date
09-Oct-1998
ICS
77.040.30 - Chemical analysis of metals
Technical Committee
E01 - Analytical Chemistry for Metals, Ores, and Related Materials
Drafting Committee
E01.20 - Fundamental Practices
Current Stage
Ref Project

Relations

Replaced By
ASTM E1306-94(2004) - Standard Practice for Preparation of Metal and Alloy Samples by Electric Arc Remelting for the Determination of Chemical Composition
Effective Date
01-May-2004
Referred By
ASTM E1806-23 - Standard Practice for Sampling Steel and Iron for Determination of Chemical Composition
Effective Date
10-Oct-1998

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ASTM E1306-94(1998)e1 - Standard Practice for Preparation of Metal and Alloy Samples by Electric Arc Remelting for the Determination of Chemical CompositionASTM E1306-94(1998)e1 - Standard Practice for Preparation of Metal and Alloy Samples by Electric Arc Remelting for the Determination of Chemical Composition
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ASTM E1306-94(1998)e1 - Standard Practice for Preparation of Metal and Alloy Samples by Electric Arc Remelting for the Determination of Chemical Composition
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
e1
Designation: E 1306 – 94 (Reapproved 1998)
Standard Practice for
Preparation of Metal and Alloy Samples by Electric Arc
Remelting for the Determination of Chemical Composition
This standard is issued under the fixed designation E 1306; 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—Footnote 1 was corrected in October 1998.
1. Scope 5. Significance and Use
1.1 This practice covers the preparation of solid samples of 5.1 This sampling practice is useful for converting chips,
reactive and refractory metals and alloys by electric arc turnings, and wires taken from ingots or other solid materials
remelting. The samples for melting may be in the form of into a homogeneous solid sample suitable for direct excitation
chips, turnings, wires, and sponge. Powdered metals need to be on an optical emission or X-ray fluorescence spectrometer. The
compacted before melting. resultant button may itself be chipped to provide samples for
1.1.1 This practice is also suitable for preparation of solid plasma emission, atomic absorption, and wet chemical analy-
samples of other metals, such as steels, stainless steels, tool sis.
steels, nickel, nickel alloys, cobalt, and cobalt alloys by electric 5.2 This practice has been used extensively for the prepa-
arc remelting. ration of zirconium, zirconium alloy, titanium, and titanium
1.2 This standard does not purport to address all of the alloy materials, and is applicable to other reactive, refractory,
safety concerns, if any, associated with its use. It is the ferrous and nonferrous alloys, such as cobalt, cobalt alloys,
responsibility of the user of this standard to establish appro- columbium (niobium), nickel, nickel alloys, stainless steels,
priate safety and health practices and determine the applica- tantalum, tool steels, and tungsten.
bility of regulatory limitations prior to use. Specific hazard
6. Interferences
statements are given in Section 9.
6.1 Test samples of known composition shall be used to
2. Referenced Documents
determine if there is any selective volatilization or segregation
2.1 ASTM Standards: of the impurity elements. Elements known to volatilize are
E 135 Terminology Relating to Analytical Chemistry for bismuth, cadium, chlorine, lead, magnesium, sodium, tellu-
Metals, Ores, and Related Materials rium, thallium, uranium, and zinc. Other elements that may
change in content are the interstitial gases, oxygen, nitrogen,
3. Terminology
and hydrogen, plus carbon, which may be added due to the
3.1 Definitions—For definitions of terms used in this prac- graphite anode. A tungsten anode may be substituted if carbon
tice, refer to Terminology E 135.
pickup is a concern. Copper contamination also may be
introduced from the melting crucible.
4. Summary of Practice
7. Apparatus
4.1 Metal chips, turnings, or wires are melted into a button
1 1
approximately 1 ⁄4 in. in diameter and approximately ⁄4-in. 7.1 Electric Arc Remelt Furnace—An apparatus suitable for
thick using an electric arc furnace. The action of the arc creates
this practice is shown schematically in Fig. 1. It shall be
agitation and mixing of the molten metal which produces a equipped as follows:
homogeneous sample.
7.1.1 Water-Cooled Upper Housing (1), approximately 6-in.
diameter and 6 ⁄4 in. high, and having a smooth, flat sealing
surface.
This practice is under the jurisdiction of ASTM Committee E-1 on Analytical
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.20 on Fundamental Practices and Measurement Traceability.
Current edition approved July 15, 1994. Published September 1994. Originally
published as E 1306 – 89. Last previous edition E 1306 – 89. A commercially available unit, including expendable parts, manufactured by
Annual Book of ASTM Standards, Vol 03.05. Cianflone Scientific Instruments Corp., Pittsburgh, PA, has been found satisfactory.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E 1306
8. Reagents and Materials
8.1 Argon, 99.99 %, gas or liquid.
1 1
8.2 Anode, graphite, ⁄2-in. diameter and 2 ⁄2 in. long with a
tapered tip.
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 An exhaust vent shall be installed over the furnace to
remove any harmful fumes that may be given off during the
melting cycle.
Legend:
10. Preparation of Apparatus
(1) Anode Housing (7) Hydraulic Jack
10.1 Initial Setup—Refer to Fig. 1.
(2) Rubber Boot (8) D-C Electrical Welder
(3) Relief Valve (9) Pressure Regulator
10.1.1 Attach the cooling water to the apparatus and adjust
(4) Inlet Fittings for Argon (10) Vacuum Pump
the flowrate to ⁄4 L/min.
(5) Outlet Fitting for Vacuum (11) Control Panel
10.1.2 Attach the argon supply and adjust the two-stage
(6) Crucible Housing (12) Power Cable
regulator output to 6 psi (41 kPa).
FIG. 1 Schematic of Electric Arc Remelt Furnace
10.1.3 Attach the vacuum pump.
10.1.4 Attach the d-c electric welder to the apparatus at the
control panel.
7.1.2 Rubber Boot (2), shall cover the anode manipulator
10.1.5 Attach the graphite anode to the manipulator assem-
assembly to prevent electrical shock.
bly.
7.1.3 The top of the housing shall be fabricated from an
10.2 Preparation of Anode—The lifetime of the anode can
electrical and thermal insulating material, such as Bakelite, and
be extended significantly by dipping it into the molten metal.
shall support the following items:
When this procedure is used, it is impe
...

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SIGNIFICANCE AND USE
4.1 These test methods for the chemical analysis of metals and alloys are primarily intended as referee methods to test such materials for compliance with compositional specifications, particularly those under the jurisdiction of ASTM Committees A01 on Steel, Stainless Steel, and Related Alloys and A04 on Iron Castings. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory under appropriate quality control practices such as those described in Guide E882.
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1.1 These test methods cover the chemical analysis of carbon steels, low-alloy steels, silicon electrical steels, ingot iron, and wrought iron having chemical compositions within the following limits:    
Element  
Composition Range, %  
Aluminum  
0.001 to 1.50  
Antimony  
0.002 to 0.03  
Arsenic  
0.0005 to 0.10  
Bismuth  
0.005 to 0.50  
Boron  
0.0005 to 0.02  
Calcium  
0.0005 to 0.01  
Cerium  
0.005 to 0.50  
Chromium  
0.005 to 3.99  
Cobalt  
0.01 to 0.30  
Columbium (Niobium)  
0.002 to 0.20  
Copper  
0.005 to 1.50  
Lanthanum  
0.001 to 0.30  
Lead  
0.001 to 0.50  
Manganese  
0.01 to 2.50  
Molybdenum  
0.002 to 1.50  
Nickel  
0.005 to 5.00  
Nitrogen  
0.0005 to 0.04  
Oxygen  
0.0001 to 0.03  
Phosphorus  
0.001 to 0.25  
Selenium  
0.001 to 0.50  
Silicon  
0.001 to 5.00  
Sulfur  
0.001 to 0.60  
Tin  
0.002 to 0.10  
Titanium  
0.002 to 0.60  
Tungsten  
0.005 to 0.10  
Vanadium  
0.005 to 0.50  
Zirconium  
0.005 to 0.15  
1.2 The test methods in this standard are contained in the sections indicated as follows:    
Sections  
Aluminum, Total, by the 8-Quinolinol Gravimetric
Method (0.20 % to 1.5 %)  
124–131  
Aluminum, Total, by the 8-Quinolinol
Spectrophotometric Method
(0.003 % to 0.20 %)  
76–86  
Aluminum, Total or Acid-Soluble, by the Atomic
Absorption Spectrometry Method
(0.005 % to 0.20 %)  
308–317  
Antimony by the Brilliant Green Spectrophotometric
Method (0.0002 % to 0.030 %)  
142–151  
Bismuth by the Atomic Absorption Spectrometry
Method (0.02 % to 0.25 %)  
298–307  
Boron by the Distillation-Curcumin
Spectrophotometric Method
(0.0003 % to 0.006 %)  
208–219  
Calcium by the Direct-Current Plasma Atomic
Emission Spectrometry Method
(0.0005 % to 0.010 %)  
289–297  
Carbon, Total, by the Combustion Gravimetric Method
(0.05 % to 1.80 %)—Discontinued 1995  
Cerium and Lanthanum by the Direct Current Plasma
Atomic Emission Spectrometry Method
(0.003 % to 0.50 % Cerium, 0.001 % to 0.30 %
Lanthanum)  
249–257  
Chromium by the Atomic Absorption Spectrometry
Method (0.006 % to 1.00 %)  
220–229  
Chromium by the Peroxydisulfate Oxidation-Titration
Method (0.05 % to 3.99 %)  
230–238  
Cobalt by the Nitroso-R Salt Spectrophotometric
Method (0.01 % to 0.30 %)  
53–62  
Copper by the Sulfide Precipitation-Iodometric
Titration Method (Discontinued 1989)  
87–94  
Copper by the Atomic Absorption Spectrometry
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279–288  
Copper by the Neocuproine Spectrophotometric
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114–123  
Lead by the Ion-Exchange—Atomic Absorption
Spectrometry Method
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132–141  
Manganese by the Atomic Absorption Spectrometry
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269–278  
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9–18  
Manganese by the Peroxydisulfate-Arsenite Titrimetric
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164–171  
Molybdenum by the Thiocyanate Spectrophotometric
Method (0.01 % to 1.50 %)  
152–163  
Nickel by the Atomic Absorption Spectrometry
Method (0.003 % to 0.5 %)  
318–327  
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Element  
Composition Range, %  
Aluminum  
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Boron  
0.001 to 0.10  
Carbon  
0.03 to 2.50  
Chromium  
0.10 to 14.0  
Cobalt  
0.10 to 14.0  
Copper  
0.01 to 2.0  
Lead  
0.001 to 0.01  
Manganese  
0.10 to 15.00  
Molybdenum  
0.01 to 10.00  
Nickel  
0.02 to 4.00  
Nitrogen  
0.001 to 0.20  
Phosphorus  
0.002 to 0.05  
Silicon  
0.10 to 2.50  
Sulfur  
0.002 to 0.40  
Tungsten  
0.01 to 21.00  
Vanadium  
0.02 to 5.50  
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Sections  
Carbon, Total, by the Combustion—
Thermal Conductivity Method—
Discontinued 1986  
125–135  
Carbon, Total, by the Combustion Gravimetric
Method—Discontinued 2012  
78–88  
Chromium by the Atomic Absorption
Spectrometry Method  
(0.006 % to 1.00 %)  
174–183  
Chromium by the Peroxydisulfate
Oxidation—Titration Method  
(0.10 % to 14.00 %)  
184–192  
Chromium by the Peroxydisulfate-Oxidation
Titrimetric Method—Discontinued 1980  
117–124  
Cobalt by the Ion-Exchange—
Potentiometric Titration Method  
(2 % to 14 %)  
52–59  
Cobalt by the Nitroso-R-Salt
Spectrophotometric Method  
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60–69  
Copper by the Neocuproine
Spectrophotometric Method  
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89–98  
Copper by the Sulfide Precipitation-
Electrodeposition Gravimetric Method  
(0.01 % to 2.0 %)  
70–77  
Lead by the Ion-Exchange—Atomic
Absorption Spectrometry Method  
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Manganese by the Periodate
Spectrophotometric Method  
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Molybdenum by the Ion Exchange–
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Phosphorus by the Alkalimetric Method  
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136–143  
Phosphorus by the Molybdenum Blue
Spectrophotometric Method  
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19–29  
Silicon by the Gravimetric Method  
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29–35  
Sulfur by the Combustion-Iodate
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Sulfur by the Chromatographic
Gravimetric Method—Discontinued 1980  
109–116  
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Vanadium by the Atomic
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Element  
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0.05 to 0.30  
Beryllium  
97.5 to 100    
Beryllium Oxide  
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0.05 to 0.30  
Copper  
0.005 to 0.10  
Chromium  
0.005 to 0.10  
Iron  
0.05 to 0.30  
Magnesium  
0.02 to 0.15  
Nickel  
0.005 to 0.10  
Silicon  
0.02 to 0.15  
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10 – 19  
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[0.008 % to 0.04 %]  
30 – 39  
Nickel by the Dimethylglyoxime Spectrophotometric Test Method
[0.001 % to 0.04 %]  
40 – 49  
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5.1 This test method for the chemical analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
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4.1 These test methods for the chemical analysis of chromium metal and ferrochromium alloy are primarily intended to test such materials for compliance with compositional specifications such as Specifications A101 and A481. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
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Element  
Composition, %  
Aluminum  
0.25 max  
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0.005 max  
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0.005 max  
Bismuth  
0.005 max  
Boron  
0.005 max  
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0.10 max  
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0.05 max  
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0.05 max  
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0.05 max  
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0.50 max  
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12.00 max  
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0.005 max  
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0.07 max  
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0.05 max  
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0.50 max  
Vanadium  
0.50 max  
Zinc  
0.005 max  
Zirconium  
0.05 max  
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10 – 20  
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Standard Practice for Sampling Copper and Copper Alloys for the Determination of Chemical Composition

SIGNIFICANCE AND USE
4.1 This practice is intended primarily for the sampling of copper and copper alloys for compliance with compositional specification requirements.  
4.2 The selection of correct test pieces and the preparation of a representative sample from such test pieces are necessary prerequisites to every analysis. The analytical results will be of little value unless the sample represents the average composition of the material from which it was prepared.
SCOPE
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1.2 Cast products may be in the form of cake, billet, wire bar, ingot, ingot bar, or casting.  
1.3 Wrought products may be in the form of flat, pipe, tube, rod, bar, shape, or forging.  
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1.5 The values stated in SI units are to be regarded as standard. The values in parentheses are given for information only.  
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ASTM E55-23(Practice)
Standard Practice for Sampling Wrought Nonferrous Metals and Alloys for Determination of Chemical Composition

ABSTRACT
This practice covers the sampling, for the determination of chemical composition of nonferrous metals and alloys that have been reduced to their final form by mechanical working; that is, by such means as rolling, drawing, and extruding. The portion selection, sample preparation, sampling details, sample size and storage, and resampling are also detailed.
SCOPE
1.1 This practice covers the sampling, for the determination of chemical composition (Note 1), of nonferrous metals and alloys that have been reduced to their final form by mechanical working; that is, by such means as rolling, drawing, and extruding.  
1.1.1 Refer to Practice E255 for copper and copper alloys.  
Note 1: The selection of correct portions of material and the preparation of a representative sample from such portions are necessary prerequisites to every analysis, the analysis being of no value unless the sample actually represents the average composition of the material from which it was selected.  
1.2 In special cases, when agreed upon by the purchaser and the manufacturer, the heat analysis may be accepted as representative of the composition of the finished product. In such cases, the identity of each heat of metal should be maintained through each stage of the manufacturing process to the final form. This method of sampling is not intended to apply under these conditions.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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SIGNIFICANCE AND USE
5.1 This test method for the chemical analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all those who use this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
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Composition Range, %  
Aluminum  
3.0–8.0  
Antimony  
0.002 max  
Cadmium  
0.025 max  
Cerium  
0.03–0.10  
Copper  
0.10 max  
Iron  
0.10 max  
Lanthanum  
0.03–0.10  
Lead  
0.026 max  
Magnesium  
0.05 max  
Silicon  
0.015 max  
Tin  
0.002 max  
Titanium  
0.02 max  
Zirconium  
0.02 max  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Included are procedures for elements in the following composition ranges:    
Element  
Composition Range, %  
Aluminum  
3.0–8.0  
Cadmium  
0.0016–0.025  
Cerium  
0.005–0.10  
Iron  
0.0015–0.10  
Lanthanum  
0.009–0.10  
Lead  
0.002–0.026  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific safety hazards statements are given in Section 8, 11.2, and 13.1.  
1.5 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.

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ASTM
ASTM E1085-22(Test Method)
Standard Test Method for Analysis of Low-Alloy Steels by Wavelength Dispersive X-Ray Fluorescence Spectrometry

SIGNIFICANCE AND USE
5.1 This test method is suitable for manufacturing control and for verifying that a product meets specifications. This test method provides rapid, multi-element determinations with sufficient accuracy to ensure product quality and to minimize production delays. The analytical performance data may be used as a benchmark to determine if similar X-ray spectrometers provide equivalent precision and accuracy, or if the performance of a particular X-ray spectrometer has changed.  
5.2 Calcium is sometimes added to steel to affect inclusion shape which enhances certain mechanical properties of steel. This test method is useful for determining the residual calcium in the steel after such treatment.  
5.2.1 Because calcium occurs primarily in inclusions, the precision of this test method is a function of the distribution of the calcium-bearing inclusions in the steel. The variation of determinations on freshly prepared surfaces will give some indication of the distribution of these inclusions.
SCOPE
1.1 This test method covers the wavelength dispersive X-ray fluorescence analysis of low-alloy steels for the following elements:    
Element  
Mass Fraction
Range, %  
Calcium  
0.001 to 0.007  
Chromium  
0.04 to 2.5  
Cobalt  
0.03 to 0.2  
Copper  
0.03 to 0.6  
Manganese  
0.04 to 2.5  
Molybdenum  
0.005 to 1.5  
Nickel  
0.04 to 3.0  
Niobium  
0.002 to 0.1  
Phosphorus  
0.010 to 0.08  
Silicon  
0.06 to 1.5  
Sulfur  
0.009 to 0.1  
Vanadium  
0.012 to 0.6  
1.1.1 Unless exceptions are noted, mass fraction ranges can be extended and additional elements can be included by the use of suitable reference materials and measurement conditions. Deviations from the published scope must be validated by experimental means. See Guide E2857 for information on validation options.  
1.2 The values stated in the International System of Units (SI) are to be regarded as standard. The values given in parentheses are mathematical conversions to other units that are provided for information only, because they may be used in older software and laboratory procedures.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 10.  
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.

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ASTM
ASTM E3346-22(Guide)
Standard Guide for Combustion, Inert Gas Fusion and Hot Extraction Instruments for use in Analyzing Metals, Ores, and Related Materials

SIGNIFICANCE AND USE
5.1 The chemical measurement processes covered by this guide are used for determination of Carbon, Sulfur, Nitrogen, Oxygen and Hydrogen in metals, ores and related materials. A test method utilizing this guidance is used to test such materials, and also form the basis for quality assurance of these materials. Thus, it is economically and scientifically critical that these instruments be understood by the laboratories that use them.  
5.2 It is assumed that all who use this guide will be trained analysts, capable of performing common laboratory procedures skillfully, and safely. It is expected that any work will be performed in a properly equipped laboratory.  
5.3 It is expected that the laboratory will prepare their own work procedures for any of the information described in this guide.  
5.4 This guide contains numerous references to “manufacturer’s recommendations”. The user of this guide is expected to refer to the instrument operation manual for the specific instrument being used or consult directly with the manufacturer to obtain instructions or recommendations.  
5.5 This guide stresses the conservation of certified reference materials (CRMs). CRMs should not be used for drift checks or conditioning measurments. Other materials should be developed and used for these operations.
SCOPE
1.1 This guide covers information for using Combustion, Inert Gas Fusion and Hot Extraction instruments to determine the mass fraction of the non-metallic elements Carbon, Sulfur, Nitrogen, Oxygen and Hydrogen in metals, ores and related materials.  
1.2 This guide does not specify all the operating conditions because of the differences among different manufacturer’s instruments. Laboratories should follow instructions provided by the manufacturer of the instrument.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 The information in this guide is contained in the sections indicated as follows:    
Sections  
Carbon/Sulfur by Combustion/Infrared Detection  
14 – 19  
Nitrogen/Oxygen by Inert Gas Fusion/Thermal Conductivity and Infrared Detection  
20 – 25  
Hydrogen by Inert Gas Fusion Instrumental Measurement and Hot Extraction/Various Detection Cell Technology  
26 – 31  
1.6 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.

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