Designation: E1010 − 16

Standard Practice for

Preparation of Disk Specimens of Steel and Iron by
Remelting for Spectrochemical Analysis1
This standard is issued under the fixed designation E1010; 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 controlled rate of flow. An arc is struck between the electrode

1.1 This practice describes the preparation of disk speci- and the sample material and is maintained until the melting is
mens of steel and iron by melting chunks, chips, drillings, complete. The molten specimen is allowed to solidify in the
turnings, wire, or powder briquets with an electric arc in an crucible in an argon atmosphere. After solidification, the
argon atmosphere. Solidification of the specimen takes place in specimen is removed from the crucible and prepared for
the crucible in an argon atmosphere. The disk obtained is spectrochemical analysis.
suitable for quantitative spectrochemical analysis. 4.2 Partial losses of some elements may be experienced
1.2 The values stated in SI units are to be regarded as during the melting of the disk specimen. This procedure, if
standard. No other units of measurement are included in this carefully followed, will provide consistent losses. Elemental
standard. losses can be determined by correlating the analysis of the
charge material with the spectrochemical analysis of the
1.3 This standard does not purport to address all of the remelted specimen.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5. Significance and Use
priate safety and health practices, and determine the applica-
5.1 Most spectrochemical instruments employed for analyz-
bility of regulatory limitations prior to use. Specific warning
ing steel and iron require a solid specimen with a flat surface
statements are given in 6.2.1, Section 8, and 10.1.2.1.
large enough for analytical excitation and measurement proce-
2. Referenced Documents dures. This practice describes a procedure for converting
unusual types of steel and iron samples to satisfactory spec-
2.1 ASTM Standards:2
trochemical specimens.
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials 6. Apparatus
E876 Practice for Use of Statistics in the Evaluation of
6.1 Melting Furnace,4consisting of a chamber that contains
Spectrometric Data (Withdrawn 2003)3
the following:
3. Terminology 6.1.1 Crucible, of copper and water-cooled, in which
samples of steel or iron are melted, then solidified to form
3.1 For definitions of terms used in this procedure, refer to
specimens for spectrochemical analysis.
Terminology E135.
6.1.2 Electrode Holder, water-cooled and of negative
4. Summary of Practice polarity, that can be moved up and down easily, and may have
provisions for circular motion and adjusting the arc gap to a
4.1 The sample of steel or iron is placed in a water-cooled
fixed spacing.
copper crucible. The furnace is flushed with argon at a
6.1.3 Viewing Window, composed of dark welding-type
glass with an inner-protective glass that is impervious to heat
1
This practice is under the jurisdiction of ASTM Committee E01 on Analytical and splatter from the molten metal.
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.01 on Iron, Steel, and Ferroalloys. 6.2 DC Electric Power Generator, to supply electric current
Current edition approved Jan. 15, 2016. Published March 2016. Originally and voltage equivalent to that required for electric arc welding.
approved in 1984. Last previous edition approved in 2009 as E1010 – 09. DOI:
10.1520/E1010-16.
It may be a rotating dc generator or a static rectifier with
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or provisions to adjust the current in the 0 A to 600 A range.
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
4
the ASTM website. Melting furnaces, manufactured by Cianflone Scientific, 228 RIDC Park West
3
The last approved version of this historical standard is referenced on Drive, Pittsburgh, PA 15275, http://www.cianflone.com, have been found suitable
www.astm.org. for this purpose.

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

1
 E1010 − 16
6.2.1 Warning—A safety interlock shall be provided to TABLE 1 Precision for Remelts of Low-Alloy Steels
prevent electrical shocks to the operator when the melting Average Standard
Relative
furnace is open. Average Standard
Number of Analysis of Deviation
Element Analysis of Deviation
Specimens Original Between
6.3 Vacuum Pump, with free air capacity of 50 L/min and Metal, %
Remelts, %
Remelts, %
Between
Remelts, %
vacuum of 350 µm, minimum.
Si 6 0.283 0.277 0.010 3.61
6 0.147 0.140 0.0063 4.50
7. Materials 6 0.010 0.010 0.0010 10.00
6 0.098 0.097 0.0042 4.33
7.1 Inert Gas, argon of at least 99.96 % purity. Mn 6 1.00 0.96 0.037 3.85
7.2 Electrode, thoriated tungsten or high-purity graphite. 6 0.95 0.95 0.055 5.79
6 0.074 0.076 0.0020 2.63
6 0.35 0.35 0.012 3.43
8. Hazards Cr 6 0.080 0.080 0.0070 8.75
6 0.044 0.046 0.0023 5.00
8.1 Operating personnel should adhere to the manufactur- 6 0.004 0.003 0.0004 13.33
er’s operating recommendations to avoid electrical shock and 6 0.491 0.486 0.0164 3.37
Mo 6 0.022 0.021 0.0012 5.71
physical harm from light and heat. See 6.2.1 and 10.1.2.1 for 6 0.006 0.006 0.00052 8.67
specific warnings. 6 0.015 0.011 0.00063 5.73
6 0.153 0.155 0.0105 6.77
9. Preparation of Samples Ni 6 0.033 0.038 0.024 63.16
6 0.020 0.016 0.0017 10.62
9.1 Remove grease from samples and dry before melting. 6 0.402 0.403 0.0082 2.03
6 0.075 0.078 0.0022 2.82
Remove other surface contaminates by suitable methods. For Cu 6 0.029 0.033 0.0019 5.76
consistent melting, fine powders, chips, drillings, turnings, or 5 0.015 0.022 0.0068 30.91
wire may be compacted in a briquetting press with 35-mm die 6 0.32 0.32 0.0098 3.06
6 0.021 0.031 0.0081 26.13
at a pressure of 2800 kgf/mm2. V 6 0.036 0.035 0.0015 4.29
6 0.012 0.015 0.00041 2.73
10. Preparation of Specimens Ti 6 0.032 0.021 0.0037 17.62
6 0.002 0.002 0.0000 0.00
10.1 Place 40 g to 50 g of sample in the crucible. Close the 6 0.083 0.066 0.0056 8.48
furnace. The melting of the sample and solidification of the Al 6 0.022 0.024 0.0025 10.42
6 0.004 0.003 0.0000 0.00
specimen may vary slightly depending on the design of the 6 0.111 0.114 0.00948 8.32
furnace and the type of metal being melted. Two suggested 6 0.038 0.040 0.0039 9.75
procedures are as follows: P 6 0.013 0.013 0.0030 23.08
6 0.012 0.013 0.0023 17.69
10.1.1 Procedure A—The following steps are programmed 6 0.010 0.011 0.0000 0.00
automatically after pressing the start button: (1) flushing of the 6 0.010 0.010 0.0019 19.00
crucible with argon for 30 s, (2) igniting the arc, (3) melting S 6 0.007 0.007 0.0010 14.29
6 0.009 0.009 0.0016 17.78
with the arc for 20 s to 45 s, (4) reduction of arc current from 6 0.024 0.023 0.0015 6.52
500 A to 250 A, (5) cooling the specimen in the crucible in inert 6 0.013 0.012 0.0027 22.50
C 5 0.127 0.110 0.030 27.27
gas for approximately 2 min, and (6) indication by light and 5 0.219 0.220 0.048 21.82
buzzer that the melt cycle is completed. When the program is 5 0.182 0.170 0.030 17.65
completed, open the furnace and remove the hot specimen with 5 0.272 0.238 0.058 24.37
magnet or forceps.
10.1.2 Procedure B—Evacuate the crucible to a pressure of
approximately 350 µm of mercury. Flush the furnace with
argon and evacuate. Reflush and evacuate a third time. Shut off NOTE 1—If the determination of carbon in the specimen is required, use
a thoriated-tungsten electrode. If the determination of tungsten or thorium
the vacuum pump and flush the furnace with argon. Turn on the is required, use a graphite electrode.
power supply and lower the electrode until an arc is struck to
the sample material (Note 1). Adjust the power supply current 11. Precision and Bias
to 500 A. Raise or lower the electrode or move it in a circular 11.1 Precision:5
motion to provide uniform melting and melt any particles that 11.1.1 Tables 1-3 show the percent standard deviations and
cling to the inside of the chamber. Melt for approximately 1 the percent relative standard deviations among disks of various
min, then turn off the power supply and raise the electrode. melted ferrous metals analyzed with both atomic emission
Allow the specimen to solidify in the crucible in the argon spectrometers and X-ray fluorescence spectrometers. The pre-
atmosphere for approximately 2 min. Open the furnace and cision data are included to serve as a guide for the precision
remove the specimen by tilting chamber. Catch the hot speci- obtainable from melted specimens prepared as described in this
men in a suitable container. practice. The data were calculated in accordance with Practice
10.1.2.1 Warning—When melting fine powders, use an E876.
initial current of 100 A until the powders appear to be well
fused. Raise the current to 300 A and complete the melting.
This prevents loss of sample because of splattering of the 5
Supporting data have been filed at ASTM International Headquarters and may
powder when the arc is first struck. be obtained by requesting Research Report RR: RR:E02-1018.

2
 E1010 − 16
TABLE 2 Precision for Remelts of Cast Iron 11.1.2 The relative standard deviations among melted speci-
Average Standard
Relative mens can be quite large. The large deviations are due to
Average Standard
Element
Number of Analysis of
Analysis of
Deviation
Deviation
element losses or enrichment during melting which can be
Specimens Original Between minimized by good melting technique, particularly for carbon,
Remelts, % Between
Metal, % Remelts, %
Remelts, % sulfur, and copper. Cleaning the crucible between melts can
Si 6 1.82 1.74 0.029 1.67 reduce contamination errors, especially when widely differing
5 0.51 0.47 0.031 6.60
5 2.10 2.07 0.042 2.03 materials are melted. The physical appearance of the melted
5 1.31 1.25 0.029 2.32 specimens will sometimes be an indication of the homogeneity.
Mn 6 0.66 0.71 0.019 2.68
5 0.53 0.52 0.015 2.88 11.2 Bias:
5 0.74 0.73 0.022 3.01
5 0.77 0.76 0.0048 0.63 11.2.1 The data in Tables 1-3 show the average analyses for
Cr 6 0.15 0.17 0.012 7.06 ferrous metals before melting and for melted specimens. While
5 0.038 0.057 0.013 22.81
5 0.33 0.36 0.022 6.11 the majority of the average analyses of melted specimens
5 0.093 0.105 0.0032 3.05 compare favorably with the average analyses of the original
Mo 6 0.022 0.023 0.0010 4.35
5 0.079 0.079 0.0024 3.04
ferrous metals, there are some precautions that need to be
Ni 6 0.09 0.09 0.0083 9.22 stated concerning this practice:
5 0.08 0.09 0.0077 8.56
5 1.22 1.20 0.016 1.33
11.2.1.1 Use of a graphite electrode increases the carbon
5 0.07 0.07 0.010 14.29 concentrations considerably. Thoriated-tungsten electrodes are
Cu 6 0.97 0.98 0.019 1.94 recommended when carbon determinations are to be made on
3 0.033 0.040 0.00079 1.98
5 0.038 0.038 0.0023 6.05 the melted specimen.
5 0.23 0.30 0.124 41.33 11.2.1.2 No statistical determinations were made for tung-
V 6 0.03 0.04 0.0019 4.75
5 0.032 0.030 0.0014 4.67 sten or thorium, however, analyses of the melted specimens
5 0.027 0.026 0.0013 5.00 indicate an increase of 0.001 % to 0.03 % tungsten when using
5 0.030 0.032 0.00064 2.00
Ti 6 0.05 0.046 0.0059 12.83
a thoriated-tungsten electrode.
5 0.026 0.019 0.0017 8.95 11.2.1.3 Copper enrichment may occur as a result of faulty
5 0.027 0.021 0.0018 8.57
5 0.04 0.040 0.0027 6.75
technique when using a circular-motion electrode holder.
P 6 0.39 0.405 0.0171 4.22 11.2.1.4 Cast iron samples tend to lose silicon during
5 0.316 0.336 0.0220 6.55
5 0.024 0.032 0.010 31.25
melting.
5 0.18 0.188 0.0218 11.60 11.2.1.5 The chromium average analysis increases for stain-
less steel materials when melted.
TABLE 3 Precision for Remelts of Stainless Steels
12. Keywords
Relative
Average Standard
Number of Analysis of
Average
Deviation
Standard 12.1 disk specimen; iron; remelt; spectrochemical analysis;
Element Analysis of Deviation
Specimens Original
Remelts, %
Between
Between
steel
Metal, % Remelts, %
Remelts, %
Si 6 0.642 0.643 0.014 2.18
6 0.472 0.470 0.0089 1.89
Mn 6 1.44 1.41 0.0117 0.83
6 1.49 1.50 0.0075 0.50
Cr 6 18.91 19.00 0.124 0.65
6 18.02 18.20 0.0884 0.49
Mo 6 0.076 0.087 0.0052 5.98
6 0.30 0.30 0.0063 2.10
Ni 6 11.52 11.44 0.0663 0.58
6 11.59 11.95 0.0455 0.38
Cu 6 0.185 0.192 0.0041 2.14
6 0.103 0.101 0.000 0.00
Sn 6 0.015 0.010 0.0004 4.00
6 0.011 0.009 0.0016 17.78
Pb 6 0.0023 0.0018 0.00041 22.78
6 0.0021 0.0019 0.0000 0.00
Co 6 0.072 0.069 0.000 0.00
6 0.144 0.149 0.000 0.00
P 6 0.018 0.018 0.0008 4.44
6 0.024 0.024 0.0016 6.67
S 6 0.018 0.017 0.0012 7.06
6 0.018 0.017 0.0013 7.65
C 5 0.018 0.020 0.014 70.00
5 0.032 0.040 0.019 47.5
Cb 6 0.731 0.725 0.033 4.55
Ta 6 0.035 0.035 0.000 0.00

3
 E1010 − 16
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