1、Designation: E1010 09Standard Practice forPreparation of Disk Specimens of Steel and Iron forSpectrochemical Analysis by Remelting1This standard is issued under the fixed designation E1010; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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 speci-mens of steel and iron by melting chunks, chi
3、ps, drillings,turnings, wire, or powder briquets with an electric arc in anargon atmosphere. Solidification of the specimen takes place inthe crucible in an argon atmosphere. The disk obtained issuitable for quantitative spectrochemical analysis.1.2 The values stated in SI units are to be regarded a
4、sstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices, and determine th
5、e applica-bility of regulatory limitations prior to use. Specific warningstatements 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 forMetals, Ores, and Related MaterialsE876 Practice for Use of Statistics in th
6、e Evaluation ofSpectrometric Data33. Terminology3.1 For definitions of terms used in this procedure, refer toTerminology E135.4. Summary of Practice4.1 The sample of steel or iron is placed in a water-cooledcopper crucible. The furnace is flushed with argon at acontrolled rate of flow. An arc is str
7、uck between the electrodeand the sample material and is maintained until the melting iscomplete. The molten specimen is allowed to solidify in thecrucible in an argon atmosphere. After solidification, thespecimen is removed from the crucible and prepared forspectrochemical analysis.4.2 Partial losse
8、s of some elements may be experiencedduring the melting of the disk specimen. This procedure, ifcarefully followed, will provide consistent losses. Elementallosses can be determined by correlating the analysis of thecharge material with the spectrochemical analysis of theremelted specimen.5. Signifi
9、cance and Use5.1 Most spectrochemical instruments employed for analyz-ing steel and iron require a solid specimen with a flat surfacelarge enough for analytical excitation and measurement proce-dures. This practice describes a procedure for convertingunusual types of steel and iron samples to satisf
10、actory spec-trochemical specimens.6. Apparatus6.1 Melting Furnace,4consisting of a chamber that con-tains the following:6.1.1 Crucible, of copper and water-cooled, in whichsamples of steel or iron are melted, then solidified to formspecimens for spectrochemical analysis.6.1.2 Electrode Holder, water
11、-cooled and of negative polar-ity, that can be moved up and down easily, and may haveprovisions for circular motion and adjusting the arc gap to afixed spacing.6.1.3 Viewing Window, composed of dark welding-typeglass with an inner-protective glass that is impervious to heatand splatter from the molt
12、en metal.6.2 D-C Electric Power Generator, to supply electric cur-rent and voltage equivalent to that required for electric arcwelding. It may be a rotating d-c generator or a static rectifierwith provisions to adjust the current in the 0 A to 600 A range.1This practice is under the jurisdiction of
13、ASTM Committee E01 on AnalyticalChemistry for Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Oct. 1, 2009. Published November 2009. Originallyapproved in 1984. Last previous edition approved in 2004
14、as E1010 84 (2004).DOI: 10.1520/E1010-09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last
15、 approved version of this historical standard is referencedon www.astm.org.4Melting furnaces, manufactured by Cianflone Scientific, 228 RIDC Park WestDrive, Pittsburgh, PA 15275, http:/, have been found suitablefor this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
16、Conshohocken, PA 19428-2959, United States.6.2.1 WarningA safety interlock shall be provided toprevent electrical shocks to the operator when the meltingfurnace is open.6.3 Vacuum Pump, with free air capacity of 50 L/min andvacuum of 350 m, minimum.7. Materials7.1 Inert Gas, argon of at least 99.96
17、% purity.7.2 Electrode, thoriated tungsten or high-purity graphite.8. Hazards8.1 Operating personnel should adhere to the manufactur-ers operating recommendations to avoid electrical shock andphysical harm from light and heat. See 6.2.1 and 10.1.2.1 forspecific warnings.9. Preparation of Samples9.1
18、Remove grease from samples and dry before melting.Remove other surface contaminates by suitable methods. Forconsistent melting, fine powders, chips, drillings, turnings, orwire may be compacted in a briquetting press with 35-mm dieat a pressure of 2800 kgf/mm2.10. Preparation of Specimens10.1 Place
19、40 g to 50 g of sample in the crucible. Close thefurnace. The melting of the sample and solidification of thespecimen may vary slightly depending on the design of thefurnace and the type of metal being melted. Two suggestedprocedures are as follows:10.1.1 Procedure AThe following steps are programme
20、dautomatically after pressing the start button: (1) flushing of thecrucible with argon for 30 s, (2) igniting the arc, (3) meltingwith the arc for 20 s to 45 s, (4) reduction of arc current from500Ato 250A, (5) cooling the specimen in the crucible in inertgas for approximately 2 min, and (6) indicat
21、ion by light andbuzzer that the melt cycle is completed. When the program iscompleted, open the furnace and remove the hot specimen withmagnet or forceps.10.1.2 Procedure BEvacuate the crucible to a pressure ofapproximately 350 m of mercury. Flush the furnace withargon and evacuate. Reflush and evac
22、uate a third time. Shut offthe vacuum pump and flush the furnace with argon. Turn on thepower supply and lower the electrode until an arc is struck tothe sample material (Note 1). Adjust the power supply currentto 500 A. Raise or lower the electrode or move it in a circularmotion to provide uniform
23、melting and melt any particles thatcling to the inside of the chamber. Melt for approximately 1min, then turn off the power supply and raise the electrode.Allow the specimen to solidify in the crucible in the argonatmosphere for approximately 2 min. Open the furnace andremove the specimen by tilting
24、 chamber. Catch the hot speci-men in a suitable container.10.1.2.1 WarningWhen melting fine powders, use aninitial current of 100 A until the powders appear to be wellfused. Raise the current to 300 A and complete the melting.This prevents loss of sample because of splattering of thepowder when the
25、arc is first struck.NOTE 1If the determination of carbon in the specimen is required, usea thoriated-tungsten electrode. If the determination of tungsten or thoriumis required, use a graphite electrode.11. Precision and Bias11.1 Precision:511.1.1 Tables 1-3 show the percent standard deviations andth
26、e percent relative standard deviations among disks of variousmelted ferrous metals analyzed with both atomic emissionspectrometers and X-ray fluorescence spectrometers. The pre-cision data are included to serve as a guide for the precisionobtainable from melted specimens prepared as described in thi
27、spractice. The data were calculated in accordance with PracticeE876.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: E02-1018.TABLE 1 Precision for Remelts of Low-Alloy SteelsElementNumber ofSpecimensAverageAnalysis ofOriginalMe
28、tal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 0.283 0.277 0.010 3.616 0.147 0.140 0.0063 4.506 0.010 0.010 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 0.0
29、12 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 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 0.0
30、75 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 26.13V660.0360.0120.0350.0150.00150.000414.292.73Ti 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 0.11
31、4 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 21.8
32、25 0.182 0.170 0.030 17.655 0.272 0.238 0.058 24.37E1010 09211.1.2 The relative standard deviations among melted speci-mens can be quite large. The large deviations are due toelement losses or enrichment during melting which can beminimized by good melting technique, particularly for carbon,sulfur,
33、and copper. Cleaning the crucible between melts canreduce contamination errors, especially when widely differingmaterials are melted. The physical appearance of the meltedspecimens will sometimes be an indication of the homogeneity.11.2 Bias:11.2.1 The data in Tables 1-3 show the average analyses fo
34、rferrous metals before melting and for melted specimens. Whilethe majority of the average analyses of melted specimenscompare favorably with the average analyses of the originalferrous metals, there are some precautions that need to bestated concerning this practice:11.2.1.1 Use of a graphite electr
35、ode increases the carbonconcentrations considerably. Thoriated-tungsten electrodes arerecommended when carbon determinations are to be made onthe melted specimen.11.2.1.2 No statistical determinations were made for tung-sten or thorium, however, analyses of the melted specimensindicate an increase o
36、f 0.001 % to 0.03 % tungsten when usinga thoriated-tungsten electrode.11.2.1.3 Copper enrichment may occur as a result of faultytechnique when using a circular-motion electrode holder.11.2.1.4 Cast iron samples tend to lose silicon duringmelting.11.2.1.5 The chromium average analysis increases for s
37、tain-less steel materials when melted.12. Keywords12.1 disk specimen; iron; remelt; spectrochemical analysis;steelTABLE 2 Precision for Remelts of Cast IronElementNumber ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviati
38、onBetweenRemelts, %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 0.038 0.057 0.013 22.815 0.33 0.36 0.022 6.115 0.093 0.105 0.0032 3.05M
39、o 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 41.33V 6 0.03 0.04 0.0019 4.755 0.032 0.030 0.0014 4.675 0.027 0.026
40、 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 8.575 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 3 Precision for Remelts of Stainless SteelsElementNum
41、ber ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 0.642 0.643 0.014 2.186 0.472 0.470 0.0089 1.89Mn 6 1.44 1.41 0.0117 0.836 1.49 1.50 0.0075 0.50Cr 6 18.91 19.00 0.124 0.656 18.02 18.20 0.088
42、4 0.49Mo 6 0.076 0.087 0.0052 5.986 0.30 0.30 0.0063 2.10Ni 6 11.52 11.44 0.0663 0.586 11.59 11.95 0.0455 0.38Cu 6 0.185 0.192 0.0041 2.146 0.103 0.101 0.000 0.00Sn 6 0.015 0.010 0.0004 4.006 0.011 0.009 0.0016 17.78Pb 6 0.0023 0.0018 0.00041 22.786 0.0021 0.0019 0.0000 0.00Co 6 0.072 0.069 0.000 0.
43、006 0.144 0.149 0.000 0.00P 6 0.018 0.018 0.0008 4.446 0.024 0.024 0.0016 6.67S 6 0.018 0.017 0.0012 7.066 0.018 0.017 0.0013 7.65C 5 0.018 0.020 0.014 70.005 0.032 0.040 0.019 47.5Cb 6 0.731 0.725 0.033 4.55Ta 6 0.035 0.035 0.000 0.00E1010 093ASTM International takes no position respecting the vali
44、dity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subj
45、ect to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquar
46、ters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standar
47、d is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).E1010 094
