1、Designation: E 1180 08Standard Practice forPreparing Sulfur Prints for Macrostructural Evaluation1This standard is issued under the fixed designation E 1180; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. 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 provides information required to preparesulfur prints (also referred to as Baumann Prints) of mostferrous alloys to r
3、eveal the distribution of sulfide inclusions.1.2 The sulfur print reveals the distribution of sulfides insteels with bulk sulfur contents between about 0.010 and 0.40weight percent.1.3 Certain steels contain complex sulfides that do notrespond to the test solutions, for example, steels containingtit
4、anium sulfides or chromium sulfides.1.4 The sulfur print test is a qualitative test. The density ofthe print image should not be used to assess the sulfur contentof a steel. Under carefully controlled conditions, it is possibleto compare print image intensities if the images are formedonly by mangan
5、ese sulfides.1.5 The sulfur print image will reveal details of the solidi-fication pattern or metal flow from hot or cold working onappropriately chosen and prepared test specimens.1.6 This practice does not address acceptance criteria basedon the use of the method.1.7 The values stated in SI units
6、are to be regarded asstandard. No other units of measurement are included in thisstandard.1.8 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 practic
7、es and determine the applica-bility of regulatory limitations prior to use. For specificprecautionary statements, see Section 9.2. Referenced Documents2.1 ASTM Standards:2E3 Guide for Preparation of Metallographic SpecimensE7 Terminology Relating to MetallographyE 340 Test Method for Macroetching Me
8、tals and AlloysE 381 Method of Macroetch Testing Steel Bars, Billets,Blooms, and ForgingsE 407 Practice for Microetching Metals and Alloys3. Terminology3.1 DefinitionsFor definitions of terms used in this prac-tice, see Terminology E7.4. Summary of Practice4.1 The sulfur print provides a means for m
9、acroscopicevaluation of the sulfur distribution in steels and cast irons bycontact printing using photographic paper soaked in an aque-ous acid solution, for example, sulfuric acid, citric acid, oracetic acid.4.2 The test specimen is usually a disk or rectangularsection, such as used in macroetch ev
10、aluations, cut from anas-cast or wrought specimen with either a transverse orlongitudinal orientation. The specimen is freshly groundsmooth and cleaned to remove cutting oils, scale, abrasives, orother contaminants. The specimen should be at room tempera-ture when sulfur printed.4.3 A sheet of photo
11、graphic paper with (usually) a mattesurface finish of appropriate size is soaked in the diluteaqueous acid solution, any excess liquid removed, and theemulsion side of the paper is placed on the ground surface ofthe specimen. After a suitable time, the paper is removed,washed in water, fixed, washed
12、 again in water, and dried as flatas possible.4.4 The distribution of sulfur in the specimen is revealed asa mirror image on the photographic paper as darkly coloredareas of silver sulfide embedded in the emulsion.5. Significance and Use5.1 The sulfur print reveals the distribution of sulfur assulfi
13、de inclusions in the specimen. The sulfur print comple-ments macroetch methods by providing an additional proce-dure for evaluating the homogeneity of a steel product.5.2 Sulfur prints of as-cast specimens generally reveal thesolidification pattern and may be used to assess the nature ofdeoxidation,
14、 that is, rimming action versus killed steel sulfurdistributions.1This practice is under the jurisdiction of ASTM Committee E04 on Metallog-raphy and is the direct responsibility of Subcommittee E04.01 on SpecimenPreparation.Current edition approved Oct. 1, 2008. Published October 2008. Originallyap
15、proved in 1987. Last previous edition approved in 2003 as E 1180 031.2For 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
16、website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 Sulfur prints will reveal segregation patterns, includingrefilled cracks, and may reveal certain physical irregularities,for example, porosity or cracking.5.4 The nature of
17、metal flow, such as in various forgingoperations, can be revealed using sulfur prints of specimens cutparallel to the metal flow direction.5.5 The sulfur print method is suitable for process control,research and development studies, failure analysis, and formaterial acceptance purposes.5.6 The inten
18、sity of the sulfur print is influenced by theconcentration of sulfur in the steel, the chemical compositionof the sulfide inclusions, the aggressiveness of the aqueous acidsolution, and the duration of the contact printing between theacid soaked emulsion coated paper and the ground surface ofthe spe
19、cimen (this time is the order of seconds rather thanminutes). Very low sulfur content steels will produce too faintan image to be useful for macrostructural evaluations. Selec-tion of appropriate printing practices including selection oftype of emulsion coated media, acid type and strength, willyiel
20、d satisfactory prints. Very faint images in the sulfur printcan be made more visible by scanning the sulfur print into aPC, and using a photo editor to increase the color saturation.Steels with compositions that produce predominantly titaniumor chromium sulfides will not produce useful images.6. Int
21、erferences6.1 The specimen must be properly cleaned, otherwise darkspots will be produced which may be incorrectly interpreted asa gross sulfide segregate.6.2 Hydrogen sulfide gas is produced while the paper is incontact with the specimen. The hydrogen sulfide is readilyabsorbed by the wet emulsion.
22、 The hydrogen sulfide reactswith the silver halides in the emulsion to lay down insolublesilver sulfide. If the specimen contains pores or cracks,hydrogen sulfide gas may become entrapped in these openingsand may produce a brown color on the paper which may beincorrectly interpreted as a gross sulfi
23、de segregate.6.3 If air is entrapped between the contacting paper andspecimen, and is not removed, a white spot may be producedon the print. Air entrapment must be quickly removed by theuse of a rubber squeegee or roller to move bubbles to the edgeof the specimen.6.4 Image blurring may result from m
24、ovement of the paperduring contact.6.5 Specimens with low sulfur contents are often pre-etchedbefore printing to expose more sulfides and enhance the image.If the pre-etchant contains sulfate ions (for example, a stainlesssteel specimen etched with Marbles reagent), the print will belightly colored,
25、 even if sulfides are not present in the steel.Such etchants should not be used for this purpose.6.6 If chromium replaces some of the manganese in thesulfide inclusions, the print intensity for a given sulfur levelwill be reduced. An image will not be obtained, irrespective ofthe sulfur content, if
26、titanium or chromium sulfides are present.7. Apparatus7.1 LightingIf the chosen photographic paper when ex-posed to the existing room light for 15 min changes from whiteto light blue and then clears back to white when processed inthe sequence of solutions, there is no need to turn off theexisting wh
27、ite lighting, and work under amber bulb lighting;never expose the paper to sunlight.7.2 Shallow Container, such as a photographic tray, isrequired to contain the dilute aqueous acid solution. Thecontainer must be large enough to soak the emulsion coatedpaper without wrinkling.7.3 Timing Device, such
28、 as used in a photographic dark-room, is helpful for timing the contact printing time, and thewashing and fixing periods.7.4 Tank, of suitable size with cool flowing water, isrequired for washing the print.7.5 Tank, or Covered Tray, to hold the fixing agent and theprint; two can be used sequentially
29、 for faster fixing when usingemulsion coated double weight fiber based paper.7.6 DryingHeated drum dryers are no longer made.Heated drying cabinets are available for fiber base prints laidhorizontally on a screen. Resin coated papers can be dried withan infra red dryer very quickly. Clothes lines an
30、d cork pegboards will also work but the prints do not dry perfectly flat.8. Reagents and Materials8.1 Photographic paper is a multilayer paper coated with agelatin emulsion containing about 80 mg per square meter ofsilver as a halide (Cl and/or Br) supported by a paper base thatis nominally single o
31、r double weight (110 or 235 g/sq. m). Thespeed and contrast characteristics are of no importance whensulfur printing. The paper base may be fibre base or resincoated. A thin layer of baryta may separate the emulsion andthe base in order to provide a more visible image. A glossyemulsion is preferred
32、to a matte emulsion if image sharpness isimportant; the problem is that a glossy emulsion may slide onthe steel surface and cause blurring. A fibre base is preferred toa resin coated base because the fibre base tends to betterconform to the steel surface; in addition it has less tendency toslip when
33、 smoothing the paper over the steel surface. Note thatphoto paper for digital photo printing contains no silver halideemulsion and is not suitable for sulfur printing. The advantageof resin coated photographic paper, over fibre base paper, isthat the paper base is sealed from contact with the dilute
34、 acid,the rapid fixer, and the water during washing; hence theprocessing time, including drying time, is much less, especiallyif double weight paper is used. Photographic paper is availablein cut sheets and rolls of various widths. Cut sheets are ideal ifthe specimen size matches the sheet size. Rol
35、l dispensed papercan be fed from a “safe” box and cut as needed. The papersheet should be 12 to 20 mm larger than the specimen aroundthe perimeter of the specimen. If the overhang of the paper istoo great then the paper will not lie tight to the edge of thespecimen.8.2 Technical or reagent grade aci
36、ds, sulfuric acid, aceticacid, citric acid, etc., are used to make the solution in which thepaper is soaked prior to contact printing; typical concentrationsof acid are 2 to 10 % sulfuric acid, 10 to 15 % acetic acid, and10 to 15 % citric acid.8.3 A commercial photographic fixing solution (rapid fix
37、ercontains ammonium thiosulfate rather than sodium thiosulfate)is used to fix the sulfur print image after contact printing andwashing. The fixer should be tested periodically to ensure thatE1180082it is still active; set aside a print in the sunlight and if theappearance changes then the fixer is d
38、epleted and should bereplaced. Used fixer contains silver and should be disposed ofin concordance with local regulations. There is not enoughsilver to justify having the silver recovered from the used fixer.9. Hazards9.1 Sulfuric acid, H2SO4, is a highly corrosive, dangerouslyreactive, strong oxidiz
39、ing agent. It reacts with water releasingsubstantial heat. Add sulfuric acid very slowly to the waterwith constant stirring. Contact with concentrated sulfuric acidmust be avoided. The dilute solution used to soak the prints isnot particularly dangerous but exposure to it should be mini-mized and ha
40、nds should be washed after any contact. The useof rubber gloves should be considered. Use tongs to handle thepaper in the soaking solution. The other acids recommendedfor sensitizing the paper are less aggressive than sulfuric acid,however, appropriate care should be taken in mixing andhandling.9.2
41、The reactions during sulfur printing are as follows:H2SO41 MnS 5 H2S 1 MnSO4(1)H2SO41 FeS 5 H2S 1 FeSO4(2)there may be some ferrous sulfide in the steel!H2S 1 2Ag Cl 5 Ag2S 1 2HCl or (3)H2S 1 2AgBr 5 Ag2Br 1 2HCl or both.WarningNote that hydrogen sulfide is released into the room. Hydro-gen sulfide
42、is toxic and needs to be exhausted from the room if more thana few samples are sulfur printed per 8 hour time period. If you can smellthe hydrogen sulfide then an exhaust system is needed.10. Sampling and Specimens10.1 Samples are generally selected in the same manner andextent as for macroetching,
43、as described in Methods E3,E 340, and E 381. Specimens are frequently prepared torepresent the entire transverse cross section, in addition,depending on the purpose of the evaluation; the longitudinalplane may be selected, and while it is usually vertical, it maybe horizontal, when required, for exa
44、mple, checking near theedge of a slab.10.2 The number, orientation, and location of specimensmay be subject to producer-purchaser agreement.10.3 Specimens should be cut in a region away from anyeffects from hot shearing or burning; unlike macroetching, thesulfur print appearance is not affected by b
45、eing within the heataffected zone (HAZ) which results from the torch cutting ofcold steel.10.4 Specimens can be thin enough for ease of handling,generally 12 to 25 mm thick, but may be thicker, especially ifbeing prepared on only one side for electrolytical macroetchingafter sulfur printing (40 to 5
46、0 mm thick). The surface to becontact printed should be freshly ground until smooth, andcarefully cleaned. Edges should be free of flash, burrs, or scale.10.5 Very smooth surfaces, such as produced by polishing,will promote slippage between the paper and disk resulting inblurred images. A 250 micron
47、 (60 grit as packaged) finishprovided by dry grinding with a hand held abrasive grit discsander, or a contact wheel belt sander is satisfactory. Using aface mill may leave tool marks that show up in the sulfur print.Using a (single) wiper insert for the final pass may leave thesurface so smooth that
48、 it must be sanded to make it roughenough for sulfur printing. A vitreous bonded abrasive surfacegrinder may be used as long as the final pass is very light andremoves only 5 micrometer. The surface should be cleanedwith methanol to remove oils and other soils. The final surfaceroughness Ra should b
49、e no less than 0.4 micrometer and maybe as large as 1.6 micrometer if the paper tends to slip tooeasily on a smoother surface.10.6 Surface preparation (see Methods E 3, E 340 andE 381) should not produce excessive cold work at the testsurface that can close up voids and cracks.11. Procedure11.1 Soak the photographic paper in the selected aqueousacid solution. The strength of the solution will depend upon theacid selected, the sulfur content of the steel and the desiredprinting time (the reaction is very rapid). AISI 10XX steelswith sulfur contents between 0.015 wt % and 0.035
