ASTM E1010-1984(2004) Standard Practice for Preparation of Disk Specimens of Steel and Iron for Spectrochemical Analysis by Remelting《再溶化法作光谱化学分析用钢铁圆盘试样的制备的标准实施规程》.pdf

1、Designation: E 1010 84 (Reapproved 2004)Standard Practice forPreparation of Disk Specimens of Steel and Iron forSpectrochemical Analysis by Remelting1This standard is issued under the fixed designation E 1010; the number immediately following the designation indicates the year oforiginal adoption or

2、, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 b

3、y melting chunks, chips, 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 This standard does not purpor

4、t 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 the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given i

5、n 6.2.1, and Section 8.2. Referenced Documents2.1 ASTM Standards:2E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data3. Terminology3.1 For definitions of terms used in this procedure, ref

6、er toTerminology E 135.4. 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 struck between the electrodeand the sample material and is maintained until the melting iscomplete. The mo

7、lten 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 losses of some elements may be experiencedduring the preparation of the disk specimen. This procedure, ifcar

8、efully followed, will provide consistent losses. Elementallosses can be determined by correlating the analysis of thecharge material with the spectrochemical analysis of theremelted specimen.5. Significance and Use5.1 Most spectrochemical instruments employed for analyz-ing steel and iron require a

9、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 satisfactory spec-trochemical specimens.6. Apparatus6.1 Melting Furnace,3consisting of a chamber thatcont

10、ains 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-cooled and of negative polar-ity, that can be moved up and down easily, and may haveprovisions for c

11、ircular motion and adjusting the arc gap to afixed spacing.6.1.3 Viewing Window, compared of dark welding-typeglass with an inner-protective glass that is impervious to heatand splatter from the molten metal.6.2 D-C Electric Power Generator, to supply electric cur-rent and voltage equivalent to that

12、 required for electric arcwelding. It may be a rotating d-c generator or a static rectifierwith provisions to adjust the current in the 0 to 600 A range.6.2.1 CautionA safety interlock shall be provided toprevent electrical shocks to the operator when the meltingfurnace is open.1This practice is und

13、er the jurisdiction of 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, 2004. Published November 2004. Originallyapproved in 1984. Last previous edi

14、tion approved in 2000 as E 1010 84 (2000).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.3Melting furnaces,

15、manufactured by Hankison Corp., Cannonsburg, PA 15317and Zeebac Inc., Berea, OH 44017, have been found suitable for this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Vacuum Pump, with free air capacity of 50 L/min andv

16、acuum of 350 m, minimum.7. Materials7.1 Inert Gas, argon of 99.96 % purity.7.2 Electrode, thoriated tungsten or high-purity graphite.8. Safety Precautions8.1 Operating personnel should adhere to the manufactur-ers operating recommendations to avoid electrical shock andphysical harm due to light and

17、heat. See 6.2.1 and 10.1.2.1 forspecific precautions.9. Preparation of Samples9.1 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 w

18、ith 35-mm dieat a pressure of 2800 kgf/mm2.10. Preparation of Specimens10.1 Place 40 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 prepared. Two sugg

19、estedprocedures are as follows:10.1.1 Procedure AThe following steps are programmedautomatically after pressing the start button: (1) Flushing of thecrucible with argon for 30 s, (2) Igniting the arc, (3) Meltingwith the arc for 20 to 45 s, (4) Reduction of arc current from500 to 250 A. (5) Cooling

20、the specimen in the crucible in inertgas for approximately 2 min, and (6) Indication 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 ofapproxima

21、tely 350 m of mercury. Flush the furnace withargon and evacuate. Reflush and evacuate 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

22、. Raise or lower the electrode or move it in a circularmotion to provide uniform 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 argonatmos

23、phere for approximately 2 min. Open the furnace andremove the specimen by tilting chamber. Catch the hot speci-men in a suitable container.10.1.2.1 CautionWhen 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 m

24、elting.This prevents loss of sample due to splattering of the powderwhen the 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 Bia

25、s11.1 Precision:411.1.1 Tables 1-3 show the percent standard deviations andthe percent relative standard deviations among disks of variousmelted ferrous metals analyzed with both optical emissionspectrometers and X-ray fluorescence spectrometers. The pre-cision data are included to serve as a guide

26、for the precisionobtainable from melted specimens prepared as described in thispractice. The data were calculated in accordance with PracticeE 876.11.1.2 The relative standard deviations among melted speci-mens can be quite large. The large deviations are due toelement losses or enrichment during me

27、lting which can beminimized by good melting technique, particularly for carbon,sulfur, 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

28、of the homogeneity.11.2 Bias:11.2.1 The data in Tables 1-3 show the average analyses forferrous 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 preca

29、utions that need to bestated concerning this practice:11.2.1.1 Use of a graphite electrode 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 fo

30、r tung-sten or thorium, however, analyses of the melted specimensindicate an increase of 0.001 to 0.03 % tungsten when using athoriated-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

31、 to lose silicon duringmelting.11.2.1.5 The chromium average analysis increases for stain-less steel materials when melted.12. Keywords12.1 disk specimen; iron; remelt; spectrochemical analysis;steel4Supporting data for this practice, obtained by cooperative testing, are includedin Research Report R

32、R: E02-1018, which is filed at ASTM Headquarters.E 1010 84 (2004)2TABLE 1 Precision for Remelts of Low-Alloy SteelsElementNumber ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAnalysis ofRemelts, %StandardDeviationBetweenRemelts, %RelativeStandardDeviationBetweenRemelts, %Si 6 0.283 0.277 0.010

33、 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 0.0070 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 0.00

34、12 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 0.029 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

35、.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 0.040 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

36、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 17.655 0.272 0.238 0.058 24.37TABLE 2 Precision for Remelts of Cast IronElementNumber ofSpecimensAverageAnalysi

37、s ofOriginalMetal, %AverageAnalysis ofRemelts, %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 0.00

38、48 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 0.0083 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 0.03

39、8 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 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.

40、024 0.032 0.010 31.255 0.18 0.188 0.0218 11.60E 1010 84 (2004)3ASTM International takes no position respecting the validity 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

41、 patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject 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

42、 either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. 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 f

43、air hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard 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 s

44、tandard 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).TABLE 3 Precision for Remelts of Stainless SteelsElementNumber ofSpecimensAverageAnalysis ofOriginalMetal, %AverageAna

45、lysis 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 0.0884 0.49Mo 6 0.076 0.087 0.0052 5.986 0.30 0.30 0.0063 2.10Ni

46、 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 0.006 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 0.00E 1010 84 (2004)4