ASTM E1180-94(1998)

Standard Practice for Preparing Sulfur Prints for Macrostructural Examination

SCOPE
1.1 This practice provides information required to prepare sulfur prints (also referred to as Baumann Prints) of most ferrous alloys to reveal the distribution of sulfide inclusions.  
1.2 The sulfur print reveals the distribution of sulfides in steels with bulk sulfur contents between about 0.005 and 0.40 weight percent.  
1.3 Certain steels contain complex sulfides that do not respond to the test solutions, for example, steels containing titanium sulfides or chromium sulfides.  
1.4 The sulfur print test is a qualitative test. The density of the print image should not be used to assess the sulfur content of a steel. Under carefully controlled conditions, it is possible to compare print image intensities if the images are formed only by manganese sulfides.  
1.5 The sulfur print image will reveal details of the solidification pattern or metal flow from hot or cold working on appropriately chosen and prepared test specimens.  
1.6 This practice does not address acceptance criteria based on the use of the method.  
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9.

General Information

• Status: Historical
• Publication Date: 09-Oct-1998
• ICS: 71.060.10 - Chemical elements
• Technical Committee: E04 - Metallography
• Drafting Committee: E04.01 - Specimen Preparation

Relations

• Replaced By: ASTM E1180-03 - Standard Practice for Preparing Sulfur Prints for Macrostructural Examination
• Effective Date: 10-May-2003
• Referred By: ASTM E2014-17 - Standard Guide on Metallographic Laboratory Safety
• Effective Date: 10-Oct-1998

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 1180 – 94 (Reapproved 1998)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
Preparing Sulfur Prints for Macrostructural Examination
This standard is issued under the fixed designation E 1180; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Summary of Practice
1.1 This practice provides information required to prepare 4.1 The sulfur print provides a means for macroscopic
sulfur prints (also referred to as Baumann Prints) of most evaluation of the sulfur distribution in steels and cast irons by
ferrous alloys to reveal the distribution of sulfide inclusions. contact printing using photographic paper, or an equivalent,
1.2 The sulfur print reveals the distribution of sulfides in soaked in an aqueous acid solution, for example, sulfuric acid,
steels with bulk sulfur contents between about 0.005 and 0.40 citric acid, or acetic acid.
weight percent.
NOTE 1—There are light weight emulsion coated papers suitable for
1.3 Certain steels contain complex sulfides that do not
sulfur printing currently on the market.
respond to the test solutions, for example, steels containing
4.2 The test specimen is usually a disk, such as used in
titanium sulfides or chromium sulfides.
macroetch evaluations, cut from an as-cast or wrought speci-
1.4 The sulfur print test is a qualitative test. The density of
men with either a transverse or longitudinal orientation. The
the print image should not be used to assess the sulfur content
disk is ground smooth and cleaned.
of a steel. Under carefully controlled conditions, it is possible
4.3 A sheet of photographic paper (or equivalent) with a
to compare print image intensities if the images are formed
(usually) matte surface finish of appropriate size is soaked in
only by manganese sulfides.
the dilute aqueous acid solution and the emulsion side of the
1.5 The sulfur print image will reveal details of the solidi-
paper is placed on the ground surface of the disk. After a
fication pattern or metal flow from hot or cold working on
suitable time, the paper is removed, washed in water, fixed,
appropriately chosen and prepared test specimens.
washed and dried.
1.6 This practice does not address acceptance criteria based
4.4 The distribution of sulfur in the disk is revealed as a
on the use of the method.
mirror image on the photographic paper as darkly colored areas
1.7 This standard does not purport to address all of the
of silver sulfide.
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 The sulfur print reveals the distribution of sulfur as
bility of regulatory limitations prior to use. For specific
sulfide inclusions in the test sample. The sulfur print comple-
precautionary statements, see Section 9.
ments macroetch methods by providing an alternative proce-
dure for evaluating the homogeneity of a steel product.
2. Referenced Documents
5.2 Sulfur prints of as-cast specimens generally reveal the
2.1 ASTM Standards:
solidification pattern and may be used to assess the nature of
E 3 Methods of Preparation of Metallographic Specimens
deoxidation, that is, rimming action versus killed steel sulfur
E 7 Terminology Relating to Metallography
distributions.
E 340 Test Method for Macroetching Metals and Alloys
5.3 Sulfur prints will reveal segregation patterns and may
E 381 Method of Macroetch Testing Steel Bars, Billets,
reveal certain physical irregularities, for example, porosity or
Blooms, and Forgings
cracking.
E 407 Test Methods for Microetching Metals and Alloys
5.4 The nature of metal flow, such as in various forging
operations, can be revealed using sulfur prints of specimens cut
3. Terminology
parallel to the metal flow direction.
3.1 Definitions: For definitions of terms used in this prac-
5.5 The sulfur print method is suitable for process control,
tice, see Terminology E 7.
research and development studies, failure analysis, and for
materials acceptance purposes.
5.6 The intensity of the sulfur print is influenced by the
This practice is under the jurisdiction of ASTM Committee E-4 on Metallog-
raphy and is the direct responsibility of Subcommittee E04.01 on Selection and
concentration of sulfur in the steel, the chemical composition
Preparation of Samples.
of the sulfide inclusions, the aggressiveness of the aqueous acid
Current edition approved Feb. 15, 1994. Published April 1994. Originally
solution, and the duration of the contact printing between the
published as E 1180 – 87. Last previous edition E 1180 – 87.
Annual Book of ASTM Standards, Vol 03.01. acid soaked emulsion coated paper and the ground surface of
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1180
the specimen. Very low sulfur content steels will produce too acid, etc., are used to make the sensitizing solution in which the
faint an image to be useful for macrostructural evaluations. paper is soaked prior to contact printing.
Selection of appropriate printing practices including selection 8.3 A commercial photographic fixing solution is used to fix
of type of emulsion coated media, acid species, and aqueous the sulfur print image after contact printing and washing.
concentration will yield satisfactory prints. Steels with compo-
9. Hazards
sitions that produce predominantly titanium sulfides or chro-
9.1 Sulfuric acid, H SO , is a highly corrosive, dangerously
2 4
mium sulfides will not produce useful images.
reactive, strong oxidizing agent. It reacts with water releasing
substantial heat. Add sulfuric acid very slowly to the water
6. Interferences
with constant stirring. Contact with concentrated sulfuric acid
6.1 The test sample must be properly cleaned, otherwise
must be avoided. The dilute solution used to soak the prints is
dark spots will be produced which may be incorrectly inter-
not particularly dangerous but exposure to it should be mini-
preted as a gross sulfide segregate.
mized and hands should be washed after any contact. The use
6.2 Hydrogen sulfide gas is produced while the paper is in
of rubber gloves should be considered. Use tongs to handle the
contact with the disk. If the disk contains pores or cracks,
paper in the soaking solution. The other acids recommended
hydrogen sulfide gas may become entrapped in these openings
for sensitizing the paper are less aggressive than sulfuric acid,
and may produce a brown color on the paper which may be
however, appropriate care should be taken in mixing and
incorrectly interpreted as a gross sulfide segregate.
handling.
6.3 If air is entrapped between the contacting paper and disk
and is not removed, a white spot may be produced on the print. 10. Sampling and Test Specimens
6.4 Image blurring may result from movement of the paper
10.1 Samples are generally selected in the same manner and
during contact which will make interpretation difficult.
extent as for macroetching, as described in Methods E 3,
6.5 Disks with low sulfur contents are often pre-etched
E 340, and E 381. Samples are normally prepared to sample the
before printing to expose more sulfides and enhance the image.
entire cross section, and are oriented either transversely or
If the etchant contains sulfate ions (for example, a stainless
longitudinally, depending on the purpose of the examination.
steel disk etched with Marble’s reagent), the print will be
10.2 The number, orientation, and loc
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