1、Designation: E1010 09E1010 16Standard Practice forPreparation of Disk Specimens of Steel and Iron byRemelting for Spectrochemical Analysis by Remelting1This standard is issued under the fixed designation E1010; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice describes the preparation of disk specimens of steel and iron by
3、 melting chunks, chips, drillings, turnings, wire,or powder briquets with an electric arc in an argon atmosphere. Solidification of the specimen takes place in the crucible in an argonatmosphere. The disk obtained is suitable for quantitative spectrochemical analysis.1.2 The values stated in SI unit
4、s are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health pra
5、ctices, and determine the applicability of regulatorylimitations prior to use. Specific warning statements are given in 6.2.1, Section 8, and 10.1.2.1.2. Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE876 Practice for
6、 Use of Statistics in the Evaluation of Spectrometric Data (Withdrawn 2003)33. Terminology3.1 For definitions of terms used in this procedure, refer to Terminology E135.4. Summary of Practice4.1 The sample of steel or iron is placed in a water-cooled copper crucible. The furnace is flushed with argo
7、n at a controlledrate of flow. An arc is struck between the electrode and the sample material and is maintained until the melting is complete. Themolten specimen is allowed to solidify in the crucible in an argon atmosphere. After solidification, the specimen is removed fromthe crucible and prepared
8、 for spectrochemical analysis.4.2 Partial losses of some elements may be experienced during the melting of the disk specimen. This procedure, if carefullyfollowed, will provide consistent losses. Elemental losses can be determined by correlating the analysis of the charge material withthe spectroche
9、mical analysis of the remelted specimen.5. Significance and Use5.1 Most spectrochemical instruments employed for analyzing steel and iron require a solid specimen with a flat surface largeenough for analytical excitation and measurement procedures. This practice describes a procedure for converting
10、unusual types ofsteel and iron samples to satisfactory spectrochemical specimens.6. Apparatus6.1 Melting Furnace,4consisting of a chamber that contains the following:1 This practice is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is
11、 the direct responsibility ofSubcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Oct. 1, 2009Jan. 15, 2016. Published November 2009March 2016. Originally approved in 1984. Last previous edition approved in 20042009as E1010 84 (2004).E1010 09. DOI: 10.1520/E1010-09.10.1520/E1
12、010-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standar
13、d is referenced on www.astm.org.4 Melting furnaces, manufactured by Cianflone Scientific, 228 RIDC Park West Drive, Pittsburgh, PA 15275, http:/, have been found suitable for thispurpose.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication
14、of what changes have been made to the previous version. Becauseit 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 versionof the standard as published by ASTM is to be consider
15、ed the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.1.1 Crucible, of copper and water-cooled, in which samples of steel or iron are melted, then solidified to form specimens forspectrochemical analysis.6.1.2 Ele
16、ctrode Holder, water-cooled and of negative polarity, that can be moved up and down easily, and may have provisionsfor circular motion and adjusting the arc gap to a fixed spacing.6.1.3 Viewing Window, composed of dark welding-type glass with an inner-protective glass that is impervious to heat ands
17、platter from the molten metal.6.2 D-CDC Electric Power Generator, to supply electric current and voltage equivalent to that required for electric arc welding.It may be a rotating d-cdc generator or a static rectifier with provisions to adjust the current in the 0 A to 600 A range.6.2.1 WarningA safe
18、ty interlock shall be provided to prevent electrical shocks to the operator when the melting furnace isopen.6.3 Vacuum Pump, with free air capacity of 50 L/min and vacuum of 350 m, minimum.7. Materials7.1 Inert Gas, argon of at least 99.96 % purity.7.2 Electrode, thoriated tungsten or high-purity gr
19、aphite.8. Hazards8.1 Operating personnel should adhere to the manufacturers operating recommendations to avoid electrical shock and physicalharm from light and heat. See 6.2.1 and 10.1.2.1 for specific warnings.9. Preparation of Samples9.1 Remove grease from samples and dry before melting. Remove ot
20、her surface contaminates by suitable methods. Forconsistent melting, fine powders, chips, drillings, turnings, or wire may be compacted in a briquetting press with 35-mm die at apressure of 2800 kgf/mm2.10. Preparation of Specimens10.1 Place 40 g to 50 g of sample in the crucible. Close the furnace.
21、The melting of the sample and solidification of the specimenmay vary slightly depending on the design of the furnace and the type of metal being melted. Two suggested procedures are asfollows:10.1.1 Procedure AThe following steps are programmed automatically after pressing the start button: (1) flus
22、hing of thecrucible with argon for 30 s, (2) igniting the arc, (3) melting with the arc for 20 s to 45 s, (4) reduction of arc current from 500A to 250 A, (5) cooling the specimen in the crucible in inert gas for approximately 2 min, and (6) indication by light and buzzerthat the melt cycle is compl
23、eted. When the program is completed, open the furnace and remove the hot specimen with magnet orforceps.10.1.2 Procedure BEvacuate the crucible to a pressure of approximately 350 m of mercury. Flush the furnace with argon andevacuate. Reflush and evacuate a third time. Shut off the vacuum pump and f
24、lush the furnace with argon. Turn on the power supplyand lower the electrode until an arc is struck to the sample material (Note 1). Adjust the power supply current to 500 A. Raise orlower the electrode or move it in a circular motion to provide uniform melting and melt any particles that cling to t
25、he inside ofthe chamber. Melt for approximately 1 min, then turn off the power supply and raise the electrode. Allow the specimen to solidifyin the crucible in the argon atmosphere for approximately 2 min. Open the furnace and remove the specimen by tilting chamber.Catch the hot specimen in a suitab
26、le container.10.1.2.1 WarningWhen melting fine powders, use an initial current of 100Auntil the powders appear to be well fused. Raisethe current to 300 A and complete the melting. This prevents loss of sample because of splattering of the powder when the arc isfirst struck.NOTE 1If the determinatio
27、n of carbon in the specimen is required, use a thoriated-tungsten electrode. If the determination of tungsten or thorium isrequired, use a graphite electrode.11. Precision and Bias11.1 Precision:511.1.1 Tables 1-3 show the percent standard deviations and the percent relative standard deviations amon
28、g disks of variousmelted ferrous metals analyzed with both atomic emission spectrometers and X-ray fluorescence spectrometers. The precision dataare included to serve as a guide for the precision obtainable from melted specimens prepared as described in this practice. The datawere calculated in acco
29、rdance with Practice E876.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR: RR:E02-1018.E1010 162TABLE 1 Precision for Remelts of Low-Alloy SteelsElement Number ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRem
30、elts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 0.283 0.277 0.010 3.616 0.147 0.140 0.0063 4.506 0.010 0.010 0.0010 10.006 0.098 0.097 0.0042 4.33Mn 6 1.00 0.96 0.037 3.856 0.95 0.95 0.055 5.796 0.074 0.076 0.0020 2.636 0.35 0.35 0.012 3.43Cr 6 0.080 0.080 0.0
31、070 8.756 0.044 0.046 0.0023 5.006 0.004 0.003 0.0004 13.336 0.491 0.486 0.0164 3.37Mo 6 0.022 0.021 0.0012 5.716 0.006 0.006 0.00052 8.676 0.015 0.011 0.00063 5.736 0.153 0.155 0.0105 6.77Ni 6 0.033 0.038 0.024 63.166 0.020 0.016 0.0017 10.626 0.402 0.403 0.0082 2.036 0.075 0.078 0.0022 2.82Cu 6 0.
32、029 0.033 0.0019 5.765 0.015 0.022 0.0068 30.916 0.32 0.32 0.0098 3.066 0.021 0.031 0.0081 26.13V 660.0360.0120.0350.0150.00150.000414.292.73Ti 6660.0320.0020.0830.0210.0020.0660.00370.00000.005617.620.008.48Al 6 0.022 0.024 0.0025 10.426 0.004 0.003 0.0000 0.006 0.111 0.114 0.00948 8.326 0.038 0.04
33、0 0.0039 9.75P 6 0.013 0.013 0.0030 23.086 0.012 0.013 0.0023 17.696 0.010 0.011 0.0000 0.006 0.010 0.010 0.0019 19.00S 6 0.007 0.007 0.0010 14.296 0.009 0.009 0.0016 17.786 0.024 0.023 0.0015 6.526 0.013 0.012 0.0027 22.50C 5 0.127 0.110 0.030 27.275 0.219 0.220 0.048 21.825 0.182 0.170 0.030 17.65
34、5 0.272 0.238 0.058 24.37TABLE 1 Precision for Remelts of Low-Alloy SteelsElement Number ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 0.283 0.277 0.010 3.616 0.147 0.140 0.0063 4.506 0.010 0.
35、010 0.0010 10.006 0.098 0.097 0.0042 4.33Mn 6 1.00 0.96 0.037 3.856 0.95 0.95 0.055 5.796 0.074 0.076 0.0020 2.636 0.35 0.35 0.012 3.43Cr 6 0.080 0.080 0.0070 8.756 0.044 0.046 0.0023 5.006 0.004 0.003 0.0004 13.336 0.491 0.486 0.0164 3.37Mo 6 0.022 0.021 0.0012 5.716 0.006 0.006 0.00052 8.676 0.015
36、 0.011 0.00063 5.736 0.153 0.155 0.0105 6.77Ni 6 0.033 0.038 0.024 63.166 0.020 0.016 0.0017 10.62E1010 163Element Number ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %6 0.402 0.403 0.0082 2.036 0.
37、075 0.078 0.0022 2.82Cu 6 0.029 0.033 0.0019 5.765 0.015 0.022 0.0068 30.916 0.32 0.32 0.0098 3.066 0.021 0.031 0.0081 26.13V 660.0360.0120.0350.0150.00150.000414.292.73Ti 6660.0320.0020.0830.0210.0020.0660.00370.00000.005617.620.008.48Al 6 0.022 0.024 0.0025 10.426 0.004 0.003 0.0000 0.006 0.111 0.
38、114 0.00948 8.326 0.038 0.040 0.0039 9.75P 6 0.013 0.013 0.0030 23.086 0.012 0.013 0.0023 17.696 0.010 0.011 0.0000 0.006 0.010 0.010 0.0019 19.00S 6 0.007 0.007 0.0010 14.296 0.009 0.009 0.0016 17.786 0.024 0.023 0.0015 6.526 0.013 0.012 0.0027 22.50C 5 0.127 0.110 0.030 27.275 0.219 0.220 0.048 21
39、.825 0.182 0.170 0.030 17.655 0.272 0.238 0.058 24.37TABLE 2 Precision for Remelts of Cast IronElement Number ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 1.82 1.74 0.029 1.675 0.51 0.47 0.03
40、1 6.605 2.10 2.07 0.042 2.035 1.31 1.25 0.029 2.32Mn 6 0.66 0.71 0.019 2.685 0.53 0.52 0.015 2.885 0.74 0.73 0.022 3.015 0.77 0.76 0.0048 0.63Cr 6 0.15 0.17 0.012 7.065 0.038 0.057 0.013 22.815 0.33 0.36 0.022 6.115 0.093 0.105 0.0032 3.05Mo 650.0220.0790.0230.0790.00100.00244.353.04Ni 6 0.09 0.09 0
41、.0083 9.225 0.08 0.09 0.0077 8.565 1.22 1.20 0.016 1.335 0.07 0.07 0.010 14.29Cu 6 0.97 0.98 0.019 1.943 0.033 0.040 0.00079 1.985 0.038 0.038 0.0023 6.055 0.23 0.30 0.124 41.33V 6 0.03 0.04 0.0019 4.755 0.032 0.030 0.0014 4.675 0.027 0.026 0.0013 5.005 0.030 0.032 0.00064 2.00Ti 6 0.05 0.046 0.0059
42、 12.835 0.026 0.019 0.0017 8.955 0.027 0.021 0.0018 8.575 0.04 0.040 0.0027 6.75P 6 0.39 0.405 0.0171 4.225 0.316 0.336 0.0220 6.555 0.024 0.032 0.010 31.255 0.18 0.188 0.0218 11.60TABLE 2 Precision for Remelts of Cast IronElement Number ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis o
43、fRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 1.82 1.74 0.029 1.675 0.51 0.47 0.031 6.605 2.10 2.07 0.042 2.035 1.31 1.25 0.029 2.32Mn 6 0.66 0.71 0.019 2.685 0.53 0.52 0.015 2.885 0.74 0.73 0.022 3.015 0.77 0.76 0.0048 0.63Cr 6 0.15 0.17 0.012 7.065 0.0
44、38 0.057 0.013 22.815 0.33 0.36 0.022 6.115 0.093 0.105 0.0032 3.05Mo 650.0220.0790.0230.0790.00100.00244.353.04Ni 6 0.09 0.09 0.0083 9.225 0.08 0.09 0.0077 8.565 1.22 1.20 0.016 1.335 0.07 0.07 0.010 14.29Cu 6 0.97 0.98 0.019 1.943 0.033 0.040 0.00079 1.985 0.038 0.038 0.0023 6.055 0.23 0.30 0.124
45、41.33V 6 0.03 0.04 0.0019 4.755 0.032 0.030 0.0014 4.675 0.027 0.026 0.0013 5.005 0.030 0.032 0.00064 2.00Ti 6 0.05 0.046 0.0059 12.835 0.026 0.019 0.0017 8.955 0.027 0.021 0.0018 8.57E1010 16411.1.2 The relative standard deviations among melted specimens can be quite large. The large deviations are
46、 due to elementlosses or enrichment during melting which can be minimized by good melting technique, particularly for carbon, sulfur, andcopper. Cleaning the crucible between melts can reduce contamination errors, especially when widely differing materials aremelted. The physical appearance of the m
47、elted specimens will sometimes be an indication of the homogeneity.11.2 Bias:11.2.1 The data in Tables 1-3 show the average analyses for ferrous metals before melting and for melted specimens. While themajority of the average analyses of melted specimens compare favorably with the average analyses o
48、f the original ferrous metals,there are some precautions that need to be stated concerning this practice:11.2.1.1 Use of a graphite electrode increases the carbon concentrations considerably. Thoriated-tungsten electrodes arerecommended when carbon determinations are to be made on the melted specime
49、n.11.2.1.2 No statistical determinations were made for tungsten or thorium, however, analyses of the melted specimens indicatean increase of 0.001 % to 0.03 % tungsten when using a thoriated-tungsten electrode.11.2.1.3 Copper enrichment may occur as a result of faulty technique when using a circular-motion electrode holder.11.2.1.4 Cast iron samples tend to lose silicon during melting.11.2.1.5 The chromium average analysis increases for stainless steel materials when melted.12. Keywords12.1 disk specimen; iron; remelt; spectrochemical analysis; stee
