Designation: E 1558 – 99 (Reapproved 2004)

Standard Guide for

Electrolytic Polishing of Metallographic Specimens1
This standard is issued under the fixed designation E 1558; 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 4.1.3 There can be a marked saving of time if many

1.1 This guide deals with electrolytic polishing as a means specimens of the same material are polished sequentially.
of preparation of specimens for metallographic purposes. 4.1.4 Electropolishing a selected area on the surface of a
Procedures are described for polishing a variety of metals. relatively large metal part can be accomplished nondestruc-
tively, that is, without the need for sectioning to remove a
NOTE 1—References (1-133)2 on electrolytic polishing will provide the piece.
reader with specific information beyond the scope of this guide.
4.1.5 Soft, single-phase metals, which may be difficult to
1.2 This standard does not purport to address all of the polish by mechanical methods, may be successfully electropol-
safety concerns, if any, associated with its use. It is the ished.
responsibility of the user of this standard to establish appro- 4.1.6 The true microstructure of a specimen can be obtained
priate safety and health practices and determine the applica- because artifacts (such as disturbed metal, scratches, and
bility of regulatory limitations prior to use. Specific safety mechanical twins) produced on the surface, even by careful
precautions are described in Section 5 and 6.3.1. grinding and mechanical polishing operations, can be removed.
These features are important in low-load hardness testing,
2. Referenced Documents X-ray diffraction studies, and in electron microscopy, where
2.1 ASTM Standards: 3 higher resolution puts a premium on undistorted metal sur-
E 7 Terminology Relating to Metallography faces.
E 407 Test Methods for Microetching Metals and Alloys 4.1.7 After electropolishing is completed, etching can often
be accomplished by reducing the voltage (generally to about
3. Terminology
one-tenth that required for polishing) for a short time before it
3.1 Definitions—All terms used in this guide are either is turned off.
defined in Terminology E 7 or are discussed in 3.2.
3.2 Definitions of Terms Specific to This Standard: NOTE 2—Not all electropolishing solutions produce good etching
results.
3.2.1 electrolytic polish (electropolish)—A method of pol-
ishing metals and alloys in which material is removed from the 4.2 Disadvantages of Electrolytic Polishing:
surface by making the metal the anode in an electrolytic bath. 4.2.1 Many of the chemical mixtures used in electropolish-
ing are poisonous or dangerous if not properly handled (see
4. Significance and Use Section 5). These hazards are similar to those involved in the
4.1 Advantages of Electrolytic Polishing: mixing and handling of etchants, see Test Methods E 407.
4.1.1 For some metals, a high quality surface finish can be 4.2.2 In multi-phase alloys, the polishing rate of each phase
produced that is equivalent to, or better than, that which can be may be different. The result may be a non-planar surface.
obtained by mechanical methods. 4.2.3 Electropolished surfaces may be slightly undulated
4.1.2 Once procedures have been established, satisfactory rather than perfectly planar and, therefore, may not be suitable
results can be obtained rapidly with reproducibility. for examination at all magnifications.
4.2.4 The rate of polishing in areas adjacent to various
inhomogeneities, such as nonmetallic inclusions and voids, is
1
This guide is under the jurisdiction of ASTM Committee E04 on Metallography usually greater than that in the surrounding matrix and tends to
and is the direct responsibility of Subcommittee E04.01 on Specimen Preparation.
Current edition approved June 1, 2004. Published July 2004. Originally approved
exaggerate the size of the inclusions and voids.
in 1993. Last previous edition approved in 1999 as E 1558 – 99. 4.2.5 Dimples, pits, and waviness limit applications involv-
2
The boldface numbers in parentheses refer to the references at the end of this ing surface phenomena, coatings, interfaces, and cracks. Edges
standard. tend to be attacked preferentially, resulting in edge rounding.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 4.2.6 Artifacts may be produced by electropolishing.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 E 1558 – 99 (2004)
4.2.7 Specimen mounting materials may react with the read and understood concerning all of the hazards and safety
electrolyte. precautions to be observed. Users should be aware of the type
4.2.8 The electropolished surfaces of certain materials may of hazards involved in the use of all chemicals used, including
be passive and difficult to etch. those hazards that are immediate, long-term, visible, invisible,
4.2.9 Metal removal rates by electropolishing are usually and with or without odors.
quite low, typically about 1 µm/min, and all of the prior 5.1.1 Consult the product labels and MSDS for recommen-
induced damage from cutting and grinding may not be re- dations concerning proper protective clothing.
moved if preparation is stopped after a 600-grit SiC grind and
electropolishing times are short. 5.1.2 All chemicals are potentially dangerous. All persons
4.2.10 A large number of electrolytes may be needed to using any electrolyte should be thoroughly familiar with all of
polish the variety of metals encountered by a given laboratory. the chemicals involved and the proper procedure for handling,
Considerable time may be required to develop a procedure for mixing, and disposing of each chemical, as well as any
a new alloy. combinations of those chemicals.
5.1.3 Table 1 includes specific safety precautions for the
5. General Safety Precautions mixing or use of some electrolytes. The user should take care
5.1 Before using or mixing any chemicals, all product labels to observe each of these specific precautions.
and pertinent Material Safety Data Sheets (MSDS) should be

TABLE 1 Electrolytes for Electropolishing

Class Use Formula Cell Voltage Time Remarks

Group I (Electrolytes Composed of Perchloric Acid and Alcohol With or Without Organic Additions)
I-1 Al and Al alloys with less than ethanol (95 %) 800 mL 30 to 80 15 to 60 s
2 percent Si distilled water 140 mL
perchloric acid (60 %) 60 mL
steels—carbon, alloy, stainless 35 to 65 15 to 60 s
Pb, Pb-Sn, Pb-Sn-Cd, Pb-Sn-Sb 12 to 35 15 to 60 s
Zn, Zn-Sn-Fe, Zn-Al-Cu 20 to 60 ...
Mg and high Mg alloys ... ... nickel cathode
I-2 stainless steel and aluminum ethanol (95 %) 800 mL 35 to 80 15 to 60 s
perchloric acid (60 %) 200 mL
I-3 stainless steel ethanol (95 %) 940 mL 30 to 45 15 to 60 s
perchloric acid (65 %) 60 mL
I-4 steel, cast iron, Al, Al alloys, Ni, ethanol (95 %) 700 mL 30 to 65 15 to 60 s one of the best formulas for
Sn, Ag, Be, Ti, Zr, U, 2-butoxy ethanol 100 mL universal use
heat-resisting alloys perchloric acid (30 %) 200 mL
I-5 steels—stainless, alloy, ethanol (95 %) 700 mL 15 to 50 15 to 60 s universal electrolyte comparable to
high-speed; Fe, Al, Zr, Pb glycerin 100 mL I-4
perchloric acid (30 %) 200 mL
I-6 Al, Al-Si alloys ethanol (95 %) 760 mL 35 to 60 15 to 60 s particularly good with Al-Si alloys
diethyl ether 190 mL
perchloric acid (30 %) 50 mL
I-7 Mo, Ti, Zr, U-Zr alloy methanol (absolute) 600 mL 60 to 150 5 to 30 s
2-butoxy ethanol 370 mL
perchloric acid (60 %) 30 mL
I-8 Al-Si alloys methanol (absolute) 840 mL 50 to 100 5 to 60 s
glycerin 125 mL
perchloric acid (65 %) 35 mL
I-9 vanadium methanol (absolute) 590 mL 30 3s three-second cycles repeated at
2-butoxy ethanol 350 mL least seven times to prevent heating
perchloric acid (65 %) 60 mL
germanium 25 to 35 30 to 60 s
titanium 58 to 66 45 s polish only
zirconium 70 to 75 15 s polish and etch simultaneously
I-10 aluminum methanol (absolute) 950 mL 30 to 60 15 to 60 s
nitric acid 15 mL
perchloric acid (60 %) 50 mL
I-11 steels—carbon, alloy, stainless methanol (absolute) 600 mL 30–40 5–60 s good all purpose electropolish
Ti, high-temperature alloys, Pb, butylcellosolve 360 mL
Mo perchloric acid 60 mL
I-12 Al and Al alloys ethanol (95 %) 1000 mL 10 2 min not good for Al-Cu and Al-Si alloys.
perchloric acid 200 mL Black film forms. Peel off after 1–1.5
min and polish 1 min more.
I-13 steel, Al, Ni, Sn, Ti, Be ethanol (95 %) 700 mL 20 20 s Mix ethanol and water, add
stainless steel butylcellosolve 100 mL perchloric acid carefully. Then, add
Al3Ni water 137 mL butylcellosolve before use.
perchloric acid 62 mL
I-14 Ni, Ag, or Cu alloys ethanol (95 %) 700 mL 70–80 15 s
Cd butylcellosolve 100 mL
perchloric acid 200 mL

2
 E 1558 – 99 (2004)

TABLE 1 Continued
Class Use Formula Cell Voltage Time Remarks
I-15 Mo and Mo alloys methanol (absolute) 600 mL 20 s Mix methanol and water, add
water 13 mL perchloric acid carefully. Add
butylcellosolve 360 mL butylcellosolve before use.
perchloric acid 47 mL
Group II (Electrolytes Composed of Perchloric Acid and Glacial Acetic Acid in Varying Proportions)
II-1 Cr, Ti, Zr, U, acetic acid (glacial) 940 mL 20 to 60 1 to 5 min good general-purpose electrolyte
Fe, steel—carbon, alloy, stainless perchloric acid (60 %) 60 mL
II-2 Zr, Ti, U, steel—carbon and alloy acetic acid (glacial) 900 mL 12 to 70 0.5 to 2 min
perchloric acid (60 %) 100 mL
II-3 U, Zr, Ti, Al, steel—carbon and acetic acid (glacial) 800 mL 40 to 100 1 to 15 min
alloy perchloric acid (60 %) 200 mL
II-4 Ni, Pb, Pb-Sb alloys acetic acid (glacial) 700 mL 40 to 100 1 to 5 min
perchloric acid (60 %) 300 mL
II-5 3 percent Si-Fe acetic acid (glacial) 650 mL ... 5 min 0.06 A/cm2
perchloric acid (60 %) 350 mL
II-6 Cr acetic acid (glacial) 1000 mL 30–50 2–3 min can lower voltage to 25 V by adding
perchloric acid 5 mL 5–15 % water.
II-7 Hf, steel—carbon and alloy acetic acid (glacial) 1000 mL ... ... Used to polish Hf wires.
perchloric acid 50 mL
Group III (Electrolytes Composed of Phosphoric Acid in Water or Organic Solvent)
III-1 cobalt phosphoric acid (85 %) 1000 mL 1.2 3 to 5 min
III-2 pure copper distilled water 175 mL 1.0 to 1.6 10 to 40 min copper cathode
phosphoric acid (85 %) 825 mL
III-3 stainless, brass, Cu and Cu water 300 mL 1.5 to 1.8 5 to 15 min copper cathode
alloys except Sn bronze phosphoric acid (85 %) 700 mL
III-4 alpha or alpha plus beta brass, water 600 mL 1 to 2 1 to 15 min copper or stainless steel cathode
Cu-Fe, Cu-Co, Co, Cd phosphoric acid (85 %) 400 mL
III-5 Cu, Cu-Zn water 1000 mL 1 to 2 10 min copper cathode
pyrophosphoric acid 580 g
III-6 steel diethylene glycol monoethyl 500 mL 5 to 20 5 to 15 min 120°F
ether
phosphoric acid (85 %) 500 mL
III-7 Al, Ag, Mg water 200 mL 25 to 30 4 to 6 min aluminum cathode, 100 to 110°F
ethanol (95 %) 380 mL
phosphoric acid (85 %) 400 mL
III-8 uranium ethanol (absolute) 300 mL ... ...
glycerin (cp) 300 mL
phosphoric acid (85 %) 300 mL
III-9 Mn, Mn-Cu alloys ethanol (95 %) 500 mL 18 ...
glycerin 250 mL
phosphoric acid (85 %) 250 mL
III-10 Cu and Cu-base alloys distilled water 500 mL ... 1 to 5 min
ethanol (95 %) 250 mL
phosphoric acid (85 %) 250 mL
III-11 stainless steel ethanol (absolute), to 1 L ... 10 min good for all austenitic heat resistant
pyrophosphoric acid 400 g alloys, 100°F plus
III-12 Mg-Zn ethanol (95 %) 625 mL 1.5 to 2.5 3 to 30 min
phosphoric acid (85 %) 375 mL
III-13 uranium ethanol (95 %) 445 mL 18 to 20 5 to 15 min 0.03 A/cm2
ethylene glycol 275 mL
phosphoric acid (85 %) 275 mL
III-14 Al-Mg alloys water 250 mL 50–60 2 min
ethanol (95 %) 380 mL
phosphoric acid (85 %) 400 mL
III-15 Cu-Pb alloys ethanol (95 %) 620 mL good up to 30 % Pb
phosphoric acid (85 %) 380 mL
III-16 Neptunium ethanol (95 %) 400 mL after 600-grit SiC, use 6-µm
glycerol 400 mL diamond on nylon before
phosphoric acid (85 %) 800 mL electropolishing.
Group IV (Electrolytes Composed of Sulfuric Acid in Water or Organic Solvent)
IV-1 stainless steel water 250 mL 1.5 to 6 1 to 2 min
sulfuric acid 750 mL
IV-2 stainless steel, Fe, Ni water 400 mL 1.5 to 6 2 to 6 min
sulfuric acid 600 mL
IV-3 stainless steel, Fe, Ni, Mo water 750 mL 1.5 to 6 2 to 10 min particularly good for sintered
sulfuric acid 250 mL Mo— Mo—32 to 80°F
0.3 to 1 min
IV-4 molybdenum water 900 mL 1.5 to 6 0.3 to 2 min particularly good for sintered
sulfuric acid 100 mL Mo—32 to 80°F

3
 E 1558 – 99 (2004)

TABLE 1 Continued
Class Use Formula Cell Voltage Time Remarks
IV-5 stainless steel water 70 mL 1.5 to 6 0.5 to 5 min
glycerin 200 mL
sulfuric acid 720 mL
IV-6 stainless steel, aluminum water 220 mL 1.5 to 12 1 to 20 min
glycerin 200 mL
sulfuric acid 580 mL
IV-7 molybdenum methanol (absolute) 875 mL 6 to 18 0.5 to 1.5 min 32 to 80°F
sulfuric acid 125 mL
IV-8 Ni-base superalloys methanol (absolute) 800 mL 30 20 s for alloy 625
sulfuric acid 200 mL
Group V (Electrolytes Composed of Chromic Acid in Water)
V-1 stainless steel water 830 mL 1.5 to 9 2 to 10 min
chromic acid 620 g
V-2 Zn, brass water 830 mL 1.5 to 12 10 to 60 s
chromic acid 170 g
Group VI (Mixed Acids or Salts in Water or Organic Solvent)
VI-1 stainless steel phosphoric acid (85 %) 600 mL ... ...
sulfuric acid 400 mL
VI-2 stainless steel water 150 mL ... 2 min 0.3 A/cm2
phosphoric acid (85 %) 300 mL
sulfuric acid 550 mL
VI-3 stainless and alloy steel water 240 mL ... 2 to 10 min 0.1 to 0.2 A/cm2
phosphoric acid (85 %) 420 mL
sulfuric acid 340 mL
VI-4 stainless steel water 330 mL ... 1 min 0.05 A/cm2
phosphoric acid (85 %) 550 mL
sulfuric acid 120 mL
VI-5 bronze (to 9 % Sn) water 450 mL ... 1 to 5 min 0.1 A/cm2
phosphoric acid (85 %) 390 mL
sulfuric acid 160 mL
VI-6 bronze (to 6 % Sn) water 330 mL ... 1 to 5 min 0.1 A/cm2
phosphoric acid (85 %) 580 mL
sulfuric acid 90 mL
VI-7 steel water 140 mL ... 1 to 5 min 1 to 5 A/cm2, 100°F plus
glycerin 100 mL
phosphoric acid (85 %) 430 mL
sulfuric acid 330 mL
VI-8 stainless steel water 200 mL ... 5 min 1 A/cm2, 80 to 120°F
glycerin 590 mL
phosphoric acid (85 %) 100 mL
sulfuric acid 110 mL
VI-9 stainless steel water 260 mL ... 30 min 0.6 A/cm2, 80 to 120°F
chromic acid 175 g
phosphoric acid (85 %) 175 mL
sulfuric acid 580 mL
VI-10 stainless steel water 175 mL ... 60 min 0.5 A/cm2, 80 to 120°F
chromic acid 105 g
phosphoric acid (85 %) 460 mL
sulfuric acid 390 mL
VI-11 stainless and alloy steel water 240 mL ... 5 to 60 min 0.5 to A/cm2, 100 to 130°F
chromic acid 80 g
phosphoric acid (85 %) 650 mL
sulfuric acid 130 mL
VI-12 tantalum hydrofluoric acid 100 mL ... 9 min graphite cathode, 0.1 A/cm2, 90 to
sulfuric acid 900 mL 100°F
VI-13 stainless steel water 210 mL ... 5 min 0.5 A/cm2, 70 to 120°F
hydrofluoric acid 180 mL
sulfuric acid 610 mL
VI-14 zinc water 800 mL ... ... 0.002 A/cm2, 70 to 100°F
chromic acid 100 g
sulfuric acid 46 mL
sodium dichromate 310 g
acetic acid (glacial) 96 mL
VI-15 stainless steel hydrogen peroxide (30 %) 260 mL ... 5 min 0.5 A/cm2 (Caution) Dangerous
(Caution)
hydrofluoric acid 240 mL
sulfuric acid 500 mL
VI-16 stainless steel water 520 mL ... ⁄ to 4 min
12 0.08 to 0.3 A/cm2
hydrofluoric acid 80 mL
sulfuric acid 400 mL

4
 E 1558 – 99 (2004)

TABLE 1 Continued
Class Use Formula Cell Voltage Time Remarks
VI-17 stainless steel water 600 mL ... ...
chromic acid 180 g
nitric acid 60 mL
hydrochloric acid 3 mL
sulfuric acid 240 mL
VI-18 bismuth glycerin 750 mL 12 1 to 5 min 0.5 6 A/cm2 (Caution) This mixture
acetic acid (glacial) 125 mL will decompose vigorously after a
nitric acid 125 mL short time. Do not try to keep.
VI-19 magnesium ethylene-glycol-monoethyl ether 900 mL 50 to 60 10 to 30 s Bath should be stirred. Cool cracked
hydrochloric acid 100 mL ice below 35°F
VI-20 molybdenum, sintered and cast methanol (absolute) 685 mL 19 to 35 20 to 35 s Mix slowly. Heat is developed. Avoid
hydrochloric acid 225 mL contamination with water. Below
sulfuric acid 90 mL 35°F.
Group VI (Mixed Acids or Salts in Water or Organic Solvent)—Continued
VI-21 titanium ethanol (95 %) 900 mL 30 to 60 1 to 6 min (Caution) Anhydrous aluminum
n-butyl alcohol 100 mL chloride is extremely dangerous to
aluminum chloride (anhydrous) 60 g handle.
(add very slowly) (Caution)
zinc chloride (anhydrous) 250 g
VI-22 uranium acetic acid (glacial) 750 mL 80 5 to 30 min The chromic acid is dissolved in the
distilled water 210 mL water before adding to the acetic
chromic acid 180 g acid. Below 35°F.
VI-23 pure zinc ethanol (95 %) 720 mL 25 to 40 0.5 to 3 min (Caution) Anhydrous aluminum
aluminum chloride (anhydrous) 50 g chloride is extremely dangerous to
(Caution) handle. Below 60°F.
zinc chloride (anhydrous) 225 g
distilled water 160 mL
n-butyl alcohol 80 mL
VI-24 zirconium. Polish and etch glycerin (Caution) 870 mL 9 to 12 1 to 10 min (Caution) will decompose on
simultaneously hydrofluoric acid 43 mL standing, dangerous if kept too long
nitric acid 87 mL
VI-25 bismuth saturated solution KI in distilled 980 mL 7 30 s polish 30 s but allow to remain in
water electrolyte until brown film is
hydrochloric acid 20 mL dissolved
VI-26 Sb methanol (absolute) 300 mL 6–10 2–4 min pure Sb. Use Pt cathode and anode
sulfuric acid 50 mL lead wires. Agitate bath. Do not
hydrochloric acid 30 mL touch polished surface with cotton.
VI-27 Sb ethanol (95 %) 30 mL good for polarized light work
glycerol 30 mL
phosphoric acid 100 mL
sulfuric acid 30 mL
VI-28 Bi water 200 mL good for polarized light work
phosphoric acid 100 mL
sulfuric acid 200 mL
VI-29 Cr water 210 mL 18 stir bath or specimen
phosphoric acid 640 mL
sulfuric acid 150 mL
VI-30 Ge methanol (absolute) 1000 mL
hydrochloric acid 10 mL
VI-31 Nb water 300 mL 40 polish to a-alumina before
sulfuric acid 100 mL electropolishing
hydrofluoric acid 100 mL
VI-32 Nb methanol (absolute) 940 mL 50–60 10 s
sulfuric acid 50 mL
hydrofluoric acid 15 mL
VI-33 Ni-base superalloy methanol (absolute) 170 mL 30 20 s for Waspaloy and IN-100 mod. Etch
hydrochloric acid 30 mL at 5 V for 4 s.
Group VII (Alkaline Electrolytes)
VII-1 gold water to 1000 mL 7.5 2 to 4 min graphite cathode
potassium cyanide 80 g
potassium carbonate 40 g
gold chloride 50 g
VII-2 silver water to 1000 mL 2.5 To 1 min graphite cathode
sodium cyanide 100 g
potassium ferrocyanide 100 g
VII-3 silver water to 1000 mL ... To 9 min graphite cathode, 0.003 to 0.009
potassium cyanide 400 g A/cm2
silver cyanide 280 g
potassium dichromate 280 g
VII-4 tungsten water to 1000 mL ... 10 min graphite cathode, 0.09 A/cm2, 100 to
trisodium phosphate 160 g 120 F
VII-5 tungsten, lead water to 1000 mL ... 8 to 10 min graphite cathode, 0.03 to 0.06 A/cm2
sodium hydroxide 100 g

5
 E 1558 – 99 (2004)

TABLE 1 Continued
Class Use Formula Cell Voltage Time Remarks
VII-6 zinc, tin water to 1000 mL 2 to 6 15 min copper cathode, 0.1 to 0.2 A/cm2
potassium hydroxide 200 g
VII-7 W water 1000 mL 5 min
sodium hydroxide 20 g
Group VIII (Mixture of Methyl Alcohol and Nitric Acid)
VIII-1 Ni, Cu, Zn, Monel, brass, methanol (absolute) 660 mL 40 to 70 10 to 60 s very useful but dangerous
Ni-chrome, stainless steel nitric acid 330 mL

5.2 Some basic suggestions for the handling and disposal of 5.6 Most electrolytes (with few exceptions) should be
electrolytes and their ingredients are as follows: mixed and stored in clean glass containers and never be in
5.2.1 When pouring, mixing, or using electrolytes, always contact with foreign materials or organic compounds. The
use the proper protective equipment (eyewear, gloves, apron, exceptions are those electrolytes containing fluorides and
and so forth). strong alkaline solutions that should be mixed and stored in
5.2.2 Use proper devices (glass or plastic) for weighing, polyethylene or other appropriate material containers. Electro-
measuring, mixing, containing, and storage of solutions. lytes must never be allowed to become concentrated by
5.2.3 When mixing electrolytes, always add reagents to the evaporation. All electrolytes should be discarded appropriately
solvent unless specific instructions indicate otherwise. as soon as they have exceeded their immediate usefulness.
5.2.4 When using an electrolyte, always avoid direct physi- 5.7 Specimens mounted in bismuth or bismuth-containing
cal contact with the electrolyte and the specimen. Use tongs or metals must not be electropolished in perchloric acid solutions
some other indirect method of handling specimens. because this mounting medium may react explosively with the
5.2.5 In general, it is good practice to work under a properly electrolyte. Likewise, bismuth or bismuth-containing alloys
designed chemical fume hood, and it is imperative with those must not be electropolished in solutions containing perchloric
electrolytes that give off noxious odors or toxic vapors. acid. Specimens mounted in organic mounting compounds,
5.2.6 Methanol is a cumulative poison hazard. Where etha- such as Bakelite, must not be electropolished in electrolytes
nol or methanol are listed as alternates, ethanol is the preferred containing perchloric acid as they may also react explosively.
solvent. Methanol should be used in a properly designed 5.8 Specific Safety Precautions for Each Group of Electro-
chemical fume hood. lytes:
5.2.7 All spills should be cleaned up and disposed of 5.8.1 The electrolytes recommended for use are classified
properly, no matter how small the spill. into eight groups. Their chemical components are listed in the
5.2.8 Properly dispose of all solutions that are not identified order of mixing. This ordering has been done to prevent
by composition and concentration. possibly dangerous reactions. Unless other instructions are
5.2.9 Store, handle, and dispose of chemicals according to specifically given, the electrolytes are intended to be used in
the manufacturer’s recommendations. Observe printed cau- the temperature range from about 65 to 80°F. Cooling may be
tions on reagent containers. necessary to maintain this range during use.
5.2.10 Information pertaining to the toxicity hazards and 5.8.2 Group I—(Electrolytes Composed of Perchloric Acid
working precautions of chemicals, solvents, acids, bases, and and Alcohol (Methanol or Ethanol) With or Without Organic
so forth, being used (such as MSDS) should be available for Additions):
rapid consultation. 5.8.2.1 These electrolytes are believed to be safe to mix and
5.3 Many of the electrolytes in the following listing can be use provided the following safety precautions are followed.
exceedingly dangerous if carelessly handled. The pertinent Only small quantities should be mixed and stored in glass-
safety precautions for each class of electrolyte should be read stoppered bottles filled to capacity. Any evaporated solvents
before any electrolyte is mixed or used. should be replaced to keep the bottle filled. Spent or exhausted
5.4 Electrolytes containing perchloric acid and acetic anhy- polishing baths are to be promptly discarded in a manner
dride are very dangerous to mix and may be unpredictable in consistent with prevailing regulations. The electrolytes are
use. Many industrial firms and research laboratories forbid the always to be protected from heat or fire.
use of such mixtures. Certain cities also have ordinances NOTE 3—In this, and all the following formulations, the term 95 %
prohibiting the use of such potentially explosive mixtures. ethanol refers to a specifically denatured alcohol which is composed of 95
These facts are considered sufficient reason for recommending parts by volume absolute ethanol and 5 parts by volume absolute
against their use. methanol. In case this formulation is not available, the use of 100 %
5.5 Mixtures of oxidizable organic compounds and power- absolute ethanol is advised. Alcohol formulations containing benzene,
gasoline, or other denaturing substances are likely to cause difficulties and
ful oxidizing agents are always potentially dangerous. After
their use is not recommended.
some use, any electrolyte will become heavily laden with ions
of the metals polished. These ions may interfere with further 5.8.3 Group II—(Electrolytes Composed of Perchloric Acid
polishing or catalyze the decomposition of the electrolyte. The and Glacial Acetic Acid):
electrolyte then must be discarded in accordance with appro- 5.8.3.1 Very little heat is developed when perchloric acid is
priate regulations. mixed with glacial acetic acid. In mixing, the perchloric acid

6
 E 1558 – 99 (2004)
should be added to the acetic with stirring. These mixtures are Chromates and dichromates cannot be safely mixed with most
normally perfectly safe to mix and use but, nonetheless, great organic liquids but can be mixed with saturated organic acids.
care should be exercised with them. Temperatures must never Care should be taken to prevent contact with the skin.
be allowed to exceed 85°F. They are flammable and must be 5.8.8 Group VII—(Alkaline Electrolytes):
guarded against fire or the evaporation of the acetic acid. 5.8.8.1 These mixtures can be grouped into two general
Plastic parts are likely to be quickly damaged by exposure to categories, those containing cyanide, and those not containing
such mixtures. cyanide.
5.8.4 Group III—(Electrolytes Composed of Phosphoric
(1) The use of cyanide by anyone not properly trained and
Acid in Water or Organic Solvents):
familiar with it is extremely dangerous. Cyanides are among
5.8.4.1 These mixtures are generally quite easy to prepare. the quickest acting and most potent poisons likely to be
In mixing, they are handled exactly as a mineral acid; namely, encountered in the laboratory. Cyanide is so quick-acting and
the acid must be slowly poured into the water or solvent with deadly that the administration of an antidote is usually inef-
constant stirring to prevent the formation of a heavy layer of fectual. Extreme care must be taken that no droplet of the
acid at the bottom of the vessel. Some solid phosphoric acids solution or crystal of the salt is ever left around where it can be
are quite energetic in their combination with water, requiring accidentally picked up and carried to the mouth.
extra care in their mixing.
(2) Solutions of the alkali hydroxides are very useful for
5.8.5 Group IV—(Electrolytes Composed of Sulfuric Acid in
the polishing of certain amphoteric metals. Their attack on the
Water or Organic Solvents):
skin is drastic, so great care should be exercised in their use.
5.8.5.1 The addition of sulfuric acid to water produces an The dissolution of alkali hydroxides, such as NaOH, in water
extremely exothermic reaction. The acid must always be produces substantial heat. Add the pellets to the water a little
poured into the water slowly and with constant stirring. bit at a time with constant stirring until the required concen-
Cooling is necessary. Great care should be taken to prevent tration is obtained. If the temperature becomes excessive, allow
spattering. Even dilute solutions of sulfuric acid strongly attack the solution to cool back to ambient before adding more
the skin or clothing. Such solutions are also very hygroscopic. hydroxide.
They vigorously attack most plastics. The mixtures of sulfuric
acid with other inorganic acids are generally more useful as 5.8.9 Group VIII—(Mixtures of Methyl Alcohol and Nitric
electrolytes. Acid):
5.8.6 Group V—(Electrolytes Composed of Chromium Tri- 5.8.9.1 Nitric acid can be mixed with methanol with appar-
oxide in Water): ent safety (mixtures with up to about 33 % nitric acid can be
5.8.6.1 The addition of crystalline chromium trioxide (CrO safely stored). This is done by adding the acid to the alcohol
3) to water is simple, since very little heat is developed. The
with careful stirring. HNO3 cannot be safely mixed and stored
resulting chromic acid is a powerful oxidant. Under certain with any higher alcohol except in very dilute solutions (for
conditions it will liberate considerable quantities of free example, do not store solutions of more than 3 % HNO3 in
oxygen. It is generally dangerous, and possibly incendiary, in ethanol). Under certain conditions, extremely unstable or
the presence of oxidizable materials. It cannot be safely mixed explosive nitro compounds, azides or fulminates can be formed
with most organic liquids, such as alcohols or glycerol. It can in alcoholic HNO3 solutions. The spontaneous decomposition
be safely mixed with certain saturated organic acids, but should of the mixture can also be catalyzed by impurities or heat. It
not be mixed with acetic acid. Chromic acid solutions cannot should always be discarded as soon as it has served its
be used in contact with plastic parts without their eventual immediate purpose. Due to its dangerous nature, it should not
destruction. Care should be taken to prevent its contact with the be employed if its use can be avoided.
skin since repeated exposure to even dilute solutions of
chromic acid or the chromates will cause persistent and painful 6. Apparatus
ulcers that are slow to heal. Chromium trioxide is a human 6.1 For the electropolishing of metal specimens in an
poison and is a carcinogen. appropriate electrolyte, a suitable electrolysis cell and a con-
5.8.7 Group VI—(Mixed Acids or Salts in Water or Organic trollable power supply are needed. Simple laboratory appara-
Solutions): tus, such as shown in Fig. 1, can be assembled to perform this
5.8.7.1 These mixtures are safe to mix and use providing the function. Many such arrangements are described in the litera-
mixing is done properly. It must be remembered that in all ture. There are also several commercially available models of
cases, the acid is added to the solvent slowly and with constant electropolishing apparatus for either laboratory or field use.
stirring. If sulfuric acid is in the formula, it is added last and 6.2 Whenever an attempt is made to polish large surface
with particular care. If hydrofluoric acid or fluorides are part of areas, the problems of obtaining sufficient current density and
a formula, polyethylene or other similar hydrofluoric acid- cooling of the specimen and electrolyte become troublesome.
resistant vessels should be used. Particular care should be taken An adequate volume of electrolyte should be used so that
to avoid skin contact with acid fluorides since exposure to localized overheating does not occur. Supplementary cooling
them, which may pass unnoticed at the time, may result in may be required. In general, electropolishing of areas larger
serious burns later. In those electrolytes containing anhydrous than 1 cm2 is not recommended for metallographic work
aluminum chloride, extreme care must be exercised. The because of the increased difficulties encountered, but it is
reaction between this compound and water is almost explosive. possible to polish larger areas.

7
 E 1558 – 99 (2004)
level must often be maintained within close limits in the
electrolytic cell. Sufficient filtering for small amounts of power
is obtained with small chokes and capacitors. When heavy
currents are needed, a better source of power is a three-phase,
full-wave, bridge recifier.
6.5 Certain electrolytes are strong etchants of the metal
when the polishing current is off. Therefore, the provision for
rapid insertion and removal of the specimen is necessary.
6.6 The electrolyte flow rate may be an important variable.
Certain electrolytes polish best when a vigorous flow rate is
employed, using special electropolishing cells, while other
electrolytes may require gentle agitation or no agitation at all.
When using pumped solutions with specially designed polish-
ing cells, the manufacturer’s practice for adjustment of the flow
rate should be followed.
6.7 The cathode material should be relatively inert in the
electrolyte and, for best results, should be more noble than the
metal or alloy being electropolished. A stainless steel cathode
is recommended for all of the electrolytes in Table 1 where no
specific recommendation is given. Other useful cathode mate-
rials include copper, nickel, graphite and platinum. The surface
area of the cathode should be much greater than that of the
anode (surface to be polished).
6.8 Additional design features that are desirable in appara-
tus for the electropolishing of metallographic specimens are as
follows:
6.8.1 Separation of the power and control portions from the
polishing cell to protect them from corrosive fumes and
solutions;
6.8.2 Meters for the continuous indication of voltage and
current;
FIG. 1 Simple Arrangement for Electropolishing 6.8.3 Polishing cycle controlled by an automatic timer;
6.8.4 Appropriate fume hood to vent gases formed while
polishing;
6.3 Many variations are possible in the design of a cell for 6.8.5 Convenient changing of electrolytes and washing and
electrolysis. Because the current density is critical, predeter- drying of the apparatus; and
mine the approximate area to be polished so that the conditions 6.8.6 Corrosion resistant parts which are in contact with
for optimum results can be achieved. This variable can be electrolyte.
controlled by the use of simple fixed masks, such as are used
in commercial units, or by the use of protecting masks of 7. Procedure
insulating paints or tapes. 7.1 The metallographer may be required to electropolish
6.3.1 The material used for the mask may be important as some metal or alloy which has not previously been encoun-
reactions with the electrolyte may occur which may simply tered. There are several general principles which can be applied
degrade the mask material, or may lead to explosions (see advantageously in these cases. The problem should be viewed
discussions of electrolyte types I, II, V, and VIII in 5). in comparison with known procedures and information gained
6.4 Suitable power sources may be batteries, rectifier power through previous experience. It is generally helpful to compare
supplies, or direct-current generators. Because as much as 150 the relationship of the major component with elements of the
V dc may be required to polish some metals, precautions must same general group in the periodic arrangement of the ele-
be taken to avoid electrical shock. The ideal power source ments, and to study the phase diagram, if available, to predict
would be a true direct current supply with a closely controlled the number of phases and their characteristics. Single-phase
voltage. When alternating-current converted to direct-current alloys are generally easier to electropolish than multi-phase
power is used, the voltage and current characteristics needed alloys. Minor alloying elements may affect the material’s
for electropolishing can be controlled only by the use of response to polishing in a given electrolyte.
resistance. One of the best ways of obtaining the power for 7.2 The conditions required for optimum polishing of a
electropolishing is to rectify the output of a variable-voltage metal in a given electrolyte can be ascertained by plotting
transformer. When a single-phase, full wave, bridge-rectifier current density versus voltage curves. The resulting curves will
circuit is used, the output current is not satisfactory for all approximate one of the two forms shown in Fig. 2. Curve I is
electropolishing unless the ripple voltage is reduced to some typical of electrolytes that either polish over a very wide range
small value by filtering. This is because a particular ionization or will not polish at all. Curve II is characteristic of electrolytes

8
 E 1558 – 99 (2004)
media are generally impervious to attack by the electrolyte (see
5.7). When mounted samples are to be electropolished, elec-
trical contact can be made through a small hole drilled through
the back of the mount into the metal.
7.5 To aid in selecting or developing an electrolyte for a
new metal or alloy, the following characteristics should be
considered:
7.5.1 The electrolyte should be somewhat viscous.
7.5.2 The electrolyte must be a good solvent of the anode
under electrolysis conditions. Insoluble products that form
adherent deposits on the face of the specimen may prevent
polishing.
7.5.3 It is desirable that the electrolyte not attack the metal
when the current is not flowing. However, this condition is not
always achieved.
7.5.4 One or more ions of large radii [example: (PO4)−3,
(ClO4)−1, or (SO 4)−2 (and occasionally certain large organic
molecules)] are usually required in electrolytes.
7.5.5 The electrolyte should be simple to mix, stable, and
safe to handle.
7.5.6 It is desirable that the electrolyte function at room
temperature and not be sensitive to temperature changes. If
electropolishing is being done on a continuing basis, the
electrolyte can be cooled by placing the cell in a water-cooled
container having a water inlet and outlet.
FIG. 2 Typical Curves for Determining Conditions for 7.6 The cathode material and size, and the anode-to-cathode
Electropolishing
spacing and orientation, are important variables. The cathode
material should be more noble than the anode material (that is,
that form an ionic film. The dotted portion of the curve is added the surface to be polished) and the cathode surface area should
in recognition of certain published data and the observation be substantially greater than the anode surface area to be
that the formation of a polishing film requires finite time. polished. Generally, the cathode and anode surfaces should be
Polishing will occur between B and C and is usually best aligned parallel to each other with a spacing of about 10–20
slightly before C. mm.
7.3 After the polishing range is determined, other constants 7.7 The depth of the specimen below the electrolyte surface
such as preparation, electrolyte flow and time can be deter- during polishing may also influence polishing results. There
mined experimentally. In the majority of cases, a mechanically should be adequate electrolyte above the area to be polished for
prepared surface, as produced by grinding up to a 600-grit best results.
silicon carbide finish, is sufficient; however, with some alloys,
7.8 Table 2 shows a listing of some of the most common
a mechanically polished surface is desirable. Metal removal
troubles likely to be encountered in electropolishing and
rates by electropolishing are low, typically around 1 µm per
suggestions for solving the problems.
minute. To remove all prior damage from grinding, either some
rough polishing should be performed after the 600-grit grind- 7.9 Table 1 contains a listing of the formulas and conditions
ing step, or the electropolishing time may be extended, which for use of electrolytes suggested for the polishing of various
may not be desirable. The surface to be electropolished should metals. Table 3 is a cross listing of the various electrolytes for
be thoroughly cleaned to obtain uniform attack by the electro- specific metals and generally for their alloys.
lyte.
7.4 Small specimens may be mounted in compression 8. Keywords
mounting media or in castable mounting media for ease in 8.1 electrolytic polishing; electropolishing; polishing; speci-
handling for mechanical preparation. Both types of mounting men preparation (metallographic)

9
 E 1558 – 99 (2004)
TABLE 2 Electropolishing Procedural Problems and Corrections
Trouble Possible Cause Suggested Correction
Center of specimen deeply etched no polishing film at center of specimen (1) increase voltage
(2) decrease agitation
(3) use more viscous electrolyte
Pitting or etching at edges of specimen too viscous or thick film ( 1) decrease voltage
(2) increase agitation
(3) use less viscous electrolyte
Sludge settling on surface insoluble anode product ( 1) try new electrolyte
(2) increase temperature
(3) increase voltage
Roughness or matte surface insufficient or no polishing film ( 1) increase voltage
(2) use more viscous electrolyte
Waviness or streaks on polished surface (1) insufficient time (1) increase or decrease agitation
(2) incorrect agitation (2) better preparation
(3) inadequate preparation (3) increase voltage and decrease time
(4) too much time
Stains on polished surface attack after polishing current is off ( 1) remove specimen while current is still on
(2) try less corrosive electrolyte
Unpolished spots (bullseyes) gas bubbles ( 1) increase agitation
(2) decrease voltage
Phases in relief insufficient polishing film ( 1) increase voltage
(2) better preparation
(3) decrease time
Pitting (1) too long polishing (1) better preparation
(2) too high voltage (2) decrease voltage
(3) decrease time
(4) try different electrolyte

TABLE 3 Suggested Electrolytes for Metals and Generally Their Alloys

Metal or Alloy Electrolyte No.
Aluminum I-1, I-2, I-4, I-5, I-6, I-8, I-10, I-12, I-13, II-3, III-7, III-14, IV-6
Aluminum-silicon alloys I-6, I-8
Antimony II-4, VI-26, VI-27
Beryllium I-4, I-13
Bismuth VI-18, VI-25, VI-28
Cadmium I-14, III-4
Cast iron I-4, II-1
Chromium II-1, II-6, VI-29, VIII-1
Cobalt I-5, II-3, III-1, III-4, VIII-1
Copper III-2, III-3, III-4, III-5, III-10, III-15, VIII-1
Copper-zinc alloys III-3, III-4, III-5, III-10, V-2, VIII-1
Copper-tin alloys III-10, VI-5, VI-6, VIII-1
Copper-nickel alloys III-3, III-10, VIII-1
Germanium I-9, VI-30
Gold VII-1
Hafnium II-7, VII-11
Iron, pure I-5, II-1, IV-2, IV-3
Iron-silicon alloys I-5, I-6, I-8, II-5
Iron-copper alloys III-3, III-4
Iron-nickel alloys I-5, II-1, II-2, II-4, IV-3, VIII-1
Lead I-1, I-5, I-11, II-4, VII-5
Magnesium I-1, III-7, III-12, VI-19
Manganese III-9
Molybdenum I-7, I-11, I-15, IV-4, IV-7, VI-20
Neptunium III-16
Nickel-chromium II-4, VIII-1
Nickel I-4, I-13, I-14, II-4, IV-2, VIII-1
Nickel aluminide I-13
Niobium VI-31, VI-32
Silicon VII-5
Silver I-14, III-7, VII-1, VII-2, VII-3
Steel, austenitic, stainless, and super alloys I-1, I-2, I-3, I-4, I-5, I-11, I-13, II-1, II-2, II-3, III-3, III-6, III-11, IV-1, IV-2, IV-3, IV-5, IV-6, IV-8, V-1, VI-1, VI-2, VI-3,
VI-4, VI-7, VI-8, VI-9, VI-10, VI-11, VI-13, VI-15, VI-16, VI-17, VI-33, VIII-1
Steel, carbon and alloy I-1, I-2, I-4, I-5, I-11, I-13, II-1, II-2, II-3, II-5, II-7, III-6, VI-3, VI-11
Tantalum VI-12
Tin I-4, I-13, VI-5, VI-6, VII-6
Titanium I-4, I-9, I-13, II-1, II-2, II-3
Tungsten VII-4, VII-5, VII-7
Uranium I-4, I-7, II-1, II-2, II-3, III-8, III-13
Vanadium I-9
Zinc I-1, I-5, III-12, V-2, VI-14, VI-23, VII-6, VIII-1
Zirconium I-4, I-7, I-9, II-2, VI-24

10
 E 1558 – 99 (2004)

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