Designation: A 561 – 71 (Reapproved 2004)

Standard Practice for

Macroetch Testing of Tool Steel Bars1
This standard is issued under the fixed designation A 561; 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.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope 5.1.1 Specimens are usually cut from hot-rolled annealed

1.1 This practice for macroetch testing has been found to be bars, but may be cut from machined or ground bars if the bars
a useful and reliable method for evaluating the quality of tool are to be finish machined or ground.
steel bars. It is used as a quality control and inspection test to 5.1.2 The specimen should be located at a sufficient distance
reveal by deep acid etching the macrostructure in specimens from the end of the bar to avoid end effects.
cut from bars and to show the presence of such conditions as 5.1.3 For ease in handling, use specimens 1⁄4 to 1⁄2 in. (6.35
pipe, cracks, porosity, segregation, or foreign material. The to 12.7 mm) thick.
etched surface is generally examined visually, but magnifica- 5.1.4 Cut specimens to expose a transverse section of the
tion up to about 103 is occasionally employed. bar; however, the test is occasionally performed on a longitu-
dinal section.
2. Referenced Documents 5.1.5 Specimens may be taken from one or both ends of a
2.1 ASTM Adjuncts: bar. Each bar may be sampled, or a few typical specimens may
Twelve Photomacrographs2 be tested as representative of a large number of bars.

3. Apparatus 6. Specimen Preparation

3.1 Etching Containers—Macroetching may be performed 6.1 In all cutting and grinding operations on the specimen,
in a vessel of borosilicate glass, porcelain, corrosion-resistant care must be excercised to avoid heating the surface to an
metals, or some other acid-resisting material. excessively high temperature. Specimens are cut from bars by
sawing, machining, abrasive wheel cutting, or other means.
4. Reagent Cutting should be controlled to prevent smearing the cut face
4.1 Etching Reagent—A solution of equal volumes of con- and masking the structure.
centrated hydrochloric acid (HCl, sp gr 1.19) and water is 6.1.1 The “as-cut” surface of a specimen may be sufficiently
commonly used for macroetching tool steels. This solution smooth to reveal the defects for which the examination is
must be used under a ventilating hood because HCl is volatile conducted. No additional surface preparation may then be
and the fumes are corrosive and irritating, although nontoxic. necessary.
The solution may be reused within limits. With use, the 6.1.2 Additional surface preparation may be required to
concentration of dissolved iron and other metals increases and remove cutting marks and to allow details to be revealed by
the acidity of the solution decreases retarding the etching etching. In such circumstances, machining, grinding, or pol-
action. Spent solution shall be replaced with fresh solution, not ishing may be necessary. Generally, the degree of surface
replenished with concentrated acid. smoothness required is greater the finer the detail that must be
resolved. When the action of the etchant is drastic, a coarser
5. Sampling surface finish may be used.
5.1 The selection of specimens for macroetch testing must 6.1.3 The surface must be free of adhering grease and oil.
be done with care for interpretations to be of value. There should be no scale or oxide on the surface which will be
examined after etching.
1
This practice is under the jurisdiction of ASTM Committee A01 on Steel, 7. Procedure
Stainless Steel and Related Alloys and is the direct responsibility of Subcommittee
A01.29 on Tool Steel.
7.1 Temperature for Macroetching—Etching characteristics
Current edition approved September 1, 2004. Published January 2005. Originally are influenced markedly by the temperature of the etchant.
approved in 1966. Last previous edition approved in 1999 as A 561 – 71 (1999). Thus, the reagent temperature should be controlled for macro-
2
Available from ASTM International Headquarters. Request Adjunct etching if comparative results are desired. Tool steels are
ADJA0561.

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 A 561 – 71 (2004)
generally macroetched at about 160°F (71°C). At this tempera- 8.1.1 Internal:
ture, the etching reaction is vigorous and solution losses 8.1.1.1 Pipe,
through evaporation are not excessive. The solution may be 8.1.1.2 Bursts,
heated on a gas or electric hot plate, by an acid-proof
immersion heater, or by steam. 8.1.1.3 Carbide (see Note 1) or alloy segregation,
7.2 Etching Time—The etching time should be sufficiently 8.1.1.4 Concentrations of nonmetallic inclusions,
long to completely reveal the structure in the specimen, yet 8.1.1.5 Porosity, and
should not be so long as to develop artifacts such as etch pits 8.1.1.6 Internal cracks or thermal flakes.
or to obscure or obliterate the structure. Generally, etching
times under 10 min or over 40 min are avoided with tool steels. NOTE 1—Carbide segregation is better determined by examination of a
The time of etching is best adjusted by trial to develop the polished surface after etching in 4 % nital solution.
degree of etching desired. Where recovery of temperature of 8.1.2 Surface and Subsurface:
the solution is slow after immersion of cold specimens,
reproducibility is enhanced by preheating the specimens in hot 8.1.2.1 Seams, laps, cracks, etc.,
water prior to immersing in the etchant. 8.1.2.2 Ingot corner segregation or cracks, and
7.3 Macroetching Technique: 8.1.2.3 Pinholes,
7.3.1 After preparation as described above, clean the speci- 8.1.3 Miscellaneous:
men of dirt and grease with a solvent, if necessary. Then place
8.1.3.1 Entrapped metallic or nonmetallic material, and
directly into the etching solution already heated to the proper
temperature, or preheat in water as in 7.2 and then transfer to 8.1.3.2 Ingot pattern (dendritic segregation, columnar grain
the hot etching bath. The purpose of preheating the specimen is structure, etc.).
to obtain better control of the etching conditions where close 8.2 Twelve photomacrographs provide a numerical rating of
reproducibility of degree of development is desired. The severity levels of porosity (8.1.1.5) and ingot pattern (8.1.3.2)
specimen must be completely immersed. that may be present in tool steel bars.
7.3.2 Moderate agitation (stirring) of the solution during 8.2.1 These conditions identified in general as porosity and
macroetching promotes uniform development by eliminating ingot pattern are described as follows:
temperature and composition gradients. Provision for agitating
8.2.1.1 Center Porosity—A center concentration of minute
the etchant may be desirable where the volume of solution is
voids related to etched out carbides, or nonmetallic inclusions,
relatively small.
7.3.3 At the end of the etching period, remove the specimen etc.
from the hot acid and rinse immediately in a stream of water. 8.2.1.2 Ring Ingot Pattern—One or more concentric rings
Flush off the sludge which forms on the surfaces of the characterized by differential etching associated with a minor
specimen during etching with the aid of a stiff brush. Then dry gradient in chemical composition or ingot solidification.
the specimen with alcohol, a clean air blast, or live steam. 8.2.2 Ratings for the conditions can be determined by
7.3.4 After drying, protect the etched surface from rusting comparing macroetched disks with these photographs.
by an application of oil, grease, glycerine, or transparent 8.2.3 The photographs are not intended as standards for
lacquer. acceptance or rejection. The numerical identity listed with each
8. Interpretation of Results figure only refers to a degree of severity. The extent that each
condition is permissible for a given application should be
8.1 Examine the etched surface visually or at up to 103
magnification to determine its structure. Note the presence, stated by the tool steel specification covering the application or
absence, and severity of the following conditions: as negotiated between the supplier and purchaser.

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Copyright by ASTM Int'l (all rights reserved); Mon Aug 4 11:02:13 EDT 2008
Downloaded/printed by
Universadad Santiago de Chile pursuant to License Agreement. No further reproductions authorized.