330 643 9076 P.
02
ASTM £340
4~ De8ignatioaE340-.1i
/",",..
Standard Test Method for
Macroetching Metals and Alloys 1
~ SWldard is issue&!under Ibe 1i.~"desi&IIWOft £340; the nWllkrlmlllt4iolc/)' roUOWIII&
onllll8l ~~II
01, I~ IIt~casc:of'~vlllOll, \he yur oflafl RVlsion. A lIumbtr in PlRnlhcsa indicalel tM year onut n:epproval.
J"~ _1100 (0) Indu:lleI an edllorlal dlanlC alnee the Ian lei'ision or reapprov~.
Thu fW rrltfhtld has .11 flppnl'Hldp "flby fl6e1IClsf/fl~e Dtp4rlflllJlJ II/~.
SlDMt1PdJj(Jr,lE, qJtcIfte}Wl' qftmJe willell
'-
]. &:ope
1.1 These tEStprocedures describe the mctnods of macl'\).
etching metals and alloys to reveal their macrostructure.
t.~ The values stated in inch-pound units are to be
JqIl'dccl as the standard. The SI equivalents of inch-pound
uniu may be approximate.
1.3 This s141ldard does nOI purport 10 address all oj the
sq{ety concerns. if any. asaociQ/ed with its use. 11 is the
TespolUibili" of 'he user of this slandtlNl lD establish appro-
priate sq/ety and h~h praaices Gild determine tire QPp/iCQ-
bility of rtplatory /imilalioras prior to use. For specific
precautlonary mtements, see 6.2, 7.1. 8.1.3, 8.~.1. 8.8.3,
8.10.1.1, and 8.13.2.
2. Wereaced Docummts
2.1 ASTM Standards:
E 3 Melbods otPreparation of Meu1losrapbic Specimeqs2
E 381 Method of Macroetch Testias. Steel Bars, Billets,
Blooms, and FOrgjnp2
J. SigRifieanee 8Dd Use
3.1 Applications of Macroelching;
3.1.1 MaCt'oetcbiDS is used. to reveal the heleJ'08Cueity of
m~ and aDoys. Mctallocraphic spceimens and chemical
analyU$ wi1l provide the necessary dc::tailcd. infonuatioD
about 9pecit'iC localities but they Clllmot live data .bout
variation Ii'om one place to aDother unless an inOt'dioat.e
n.umber of specimens are taken.
3. J.2 MacroetdIing, on the other hand, win provide infor-
mation ODvariations in (1) strUcture, such as pain size, flow
liftCS, columnar strUCture, dendriu:s, ctC.; (2) variations in
ehemicaJ composition as evidenced by aqreptioo, carbide
and fmite banding, coring, iaclusioDs, aDd depth ot carbur-
izatioD or de<:arburizalion, The iDfonnation provided about
variations in cbemical composition is stricdy qualitative but
the location ot extremes in 5eltCption wiD be shown. Chem-
ical analya or other 111C&DS of ddcfminiq the cbemiC411
composition would bave \0 be performed to delennine the
ureat of variation. MacroetchiPB win also show the pI9:IJCC
of discontinuities and voids, such as scams, haps, porosity,
fiaJcea,bums. extrusion rupture, c:rac:ks,etc.
F\eaIt
AM[;AICANSOCl61V FOR 'niSTIIiGIANO WoTERtAlS
1918R111\t'SI PNlhlphI.
"0m 11IIAn
P'1tl~
e...k oIl'&N S1BncIarda.C--.hr
1I/IOtIoIO\t1ft1110""".nl..l!Ibtned ., ..'I_a.
~
1ft1M nut IIIS«IQI\
III. cIosicn.lion inclicawllle ~
or
"
CtWt.ruft/1r~Dol) 11Idfx 0/ SP«lI1cDlIMI tZll4
b_lJIioplN ")lI~ De(JIIIImenrqf1Jt{tlll'.
3.1.3 Other applications of macroetchin& in the fabrication
of metals are the study ofweJd structure, definition of weld
penetration. dilution of filJer metal by base metals, CD~P-
ment of flux, porosity, and cracks in weld and beat affected
z0!1es, etc. .It is also used ia the beat-treating sbop to deter-
mIne location of hard or $Oft spot$, 10Ri marks, quencbinl
cmcks. c:ase depth in shaDow-hardening steels, case depth in
carburization of dies, effectiveness of Stop.olf coatings in
carburWition, etc. In the machine shop, it caD be ~sed for the
detenninaUoI1 of BrindiDs cracks in tools and dies.
3.1.4 Macroetching is used extcDSively for Q\1atity control
in the steel industry, to d.etennine the lone ora beat in billetS
with ~t ~.inclusions, searega~on. and stt1u:rure. FOrJe
shops, 111addition, Q$C macroetcblD! to revt:aJ flow liDes in
setting up the best forains practice, die desip, aDd metal
flow. For an examp!.c of the use oftnaerOetching in the steel
forging industry see Method E 381. FotSina shops and
foundries also use macroetching to determine the presence of
internal faultS and surfice defect5. Tbe copper industry uses
macroetching fot control of surface porosity in wire bar. In
the alummum induatty,naacroetchinsis &&SOd to evaluate
extrusions as well as the oaher pzoducts such as forgings,
sheets, etc. Defects sllCh aa corin& cnwkA, and porthole die
welds are identified.
4. SampllDa
4.1 Ai in any method of e~aminati011. sampling is very
imp011aI1t When mamctehiq is used 10 solve a problem.
tbo problem itself Jarply dictates the source ofUlo sample as
to the location on the work piece and the stage of mallufac.
ture: for example, when Jooking for pipe, the sample should
represent the top of the ingot. or when looIcinS fOr bursts or
Sakes. the sample should be taken as SOODafter hot working
possible.
" 4.2 When macroetching is use4 as an inspection proce.
dure, aampJin* ousht to ~ done in an early stage of
manufactunn& so that ir the material proves faulty, no
wastefuj unnecessary work is dOQe.However, the sample
~ould not be taken so early that f~rtber workin. can
mtroduce serious defects. In the steel industry, for exampl~
the sample is us\l81JytakeD afterInaotbreakdownand after
most Cbanc:esof bunU or Oakes occurring have passed.
Billets or blooms going into small size. are 9ampJed afttr
initial b:\:akdown. Material goinS into f"orsiDibill~ or die
blocks .is sampled nw finish size. Samplins may be done
sySICmahca1)y or on I random basis.
4.3 Samples may be c:oJcicut trom 1I\e source by any
convenient fashian; saws and abrasive cutoff wheels are
p<U1icwarlyeffective.The use of torch cutting or hot cutting
... __ ____
-- --- --- 0-

ASTM £340 ~! II D?S'S10 D55S0as D~T II
41 E 340
shouldbe used only when nccossary to cut II sample from a
large piece. The sample theD is sectioned weD away (rom the
hot-cut sudace. An examp1e of permissible use of torch
cuttinC is the excisina of a pjcc:c from a larBe plate and then
cutUag a sample for macroetchius4 to 5 in. (102 to 121 mm)
away from the torcb-cut edge.
4.4 Some common methods of sampJiliJ, listed by JOu.rce,
lilt as follows:
4.5 Bi/lels, Blooms. lWi Hot-Rolled Products-Dilks ~
usually cul from these products near tbe end. Samples cut
too olose to the end, however. may bave false structU1'tS
because of fish-tailing. Disks from luge blooms are some-
times cut into smaller pieces for ease in handling.
4.5.1 FOTgi"gs (lnd &trus;ons-Disks cut 1raD8VeJWto
the 10nB dimension win Sbow Oakes. bursts, etc. Foraines
may also be eut parallel to the long dimension to show flow
lines. In complicated forgings. some thought wiIJ have to be
given to the proper method of cumn. 10 as to show Oow
lines. Macroctchiq of an unprepared specimm will show
surface defects such as shuts. &1&,scams, etc. In extrusions,
corina and ~arw grain. are more commonly Cound in the
back end of the CJt1l'ugon.
4.5.2 Sheets (pia Pldles-A Mfidentlylargc" sample
sMuld be taleen when loolciftS for surface defects. An ideal
length would be the cimunference of the IBst roll, but thir
may be inconlleniendy Ion&- Several samPles tOtalinJ some
given fraction of thc circumferencc can be used; however.
there is always a chance then tbat a defect arising from faulty
rolls would not be deteCted. When _kins infonnation on
laminations. a transverse section is u=red. In many cases,
however, to reduce the size of the specimen. only a section
out of the center of the plate may be taken.
4.5.3 We/dmmts-A. disk cut perpendicular to the diree.
tiOI! of weldinr will show weld J)CI1etratio.D,heat affected
zone, structure, etc. CatdUI preparation is usually rewarded
wi1h highly detailed muc:turcs givins . lup: amount of
information. WeJch ;DIIOlvingdissimilar metals will produce
problems in etching. The best method is to et~ the least
eorrosion-resistant portion first and the more ressstUl p0r-
tion afterwards. Occasionally an intermediary etcbaz1t may
be required. The boundaricJ betweeD ctdu:d and unetl::hed
portion will Aive an idea of weld pe»eU'lUion and dilution.
4.5.4 Casling,s-Cut the specimen to display the defea or
feature being sought.
4.5.5 Machined tl1Vi G,ormd Parts-When looking for
Grindio&CTadts. etc., the swfac:c iuelf is used as a sample.
Because the machined or ground part is often the finished
part, it may be undesirable to immure the part in acid. lu
this case, other methods such as dye pe.neuant methodi may
be more desirable.
S. Prepal18lion
5.1 Sample pRparanon need Dot be elaborate. Any
metbod of Pre3eDUng a smooth sudace with a minimum
amount of cold work win be satisfactory. Disks may be faced
on a lathe or a shaper. The usual procedure is to take a
rouJhinl cut, Chen a finish cut. This wiD aeneme a smoow
surface aDd remove cold wort from prior operations. Sbarp
tools are necessary to produce a ~ gpecimen. Grinding is
usually coDducted in the same manner. using rree-cutting
wheels and light finlshinl ~ts. When /inti deW! is requiRd,
pJrichl by lire AiDencan SocietyFor TetiDS .t ifateriaii"--
11 Nov 05 15:35:44 1998
330 643 9076 P.03
the specimen should be around down througb the series or
metallographic papers (see Methods E 3). Wbere Dece&S8IY,
det4ilS ate Biven in the tabulation of procedures.
5.2 Alter swface preparation, the sample is cleaned care.
fully with s\liable &01~ta. Any grease, 011,or other residue
win produce \1nevea auadt. Once cleaned, care should be
taken not to touch the sample surface or contaminate it in
any way.
6. SoludODl
6.1 The 'solutions used for macroetching are given in the
tables listed ullder each ailoy. In most aI5eS a good grade of
reapnt should be \1SCdbut Deed Dot be chemically pure or of
analytical quality. The so-called tecl1nical srades are usua11y
satisfactory. Tbe soll11ion should be clean and clear. free of
sUlPCnded particles, scum, etc.
6.2 Caution must be observed in n1ixin&. Many of the
etchanta .u'e stroDB acid!. In all cases, the various cbemical.s
should be added slowly to the water or solvent wmle stiMing.
In the cases where hydrofluoric acid is used, che solution
should be mixed and used il'l polyethylene vesseJs.
Non! 1: C.1IIioa-HydrofluorU:ICid sho\dci lIot be allowed (0
OQ(\1a~1tbe slQQlinee It can calle PJlinM serious ulcers irllot wllSbcd ofT
.
JD'llIIcdlarely.
,. ProcedUJe
1.1 Many otthe solutions are auressive and may dve oir
irritating and COI.T09ivefumes. Etching should be done in a
wcJl-ventilated room, preferabJy under a fume hood. The
solution should be mixed and placed in a COnoSiODresistant
tray or dish and broulht to the operating lemperature. The
spceimcn or specimcna sbould be placed in II1my of stainless
steel screen or on IOme non-rcactive suppart. Glass rods
often are placed on the bottom of the acid eonlainer and the
specimens laid directly on the rods. When etching is com-
plC1Cd,remove the specimens from the dish taking gcat caR
not to toucl1 the etched surface. When desmutting is rc.
quircd, dip tbe specimen iato IIsecond solulitln. After rinsing
the specimen with bot water, blow dry with clean com-
I"ressed air.
7.2 In the case of large specimens, such as inscn sections,
swabbins may be &heoDlypractical method of mal::roetehing.
Saturate a llU'8Cwad ofcouon beld in stainless 5\ee1or nickel
tongs wi1h the etchant IIKI sweep over the surface of me
specimen. An effort .houJd be made to wet the entire surface
as soon as possible. After the iDi1ial wettins. keep die swab
saturated with solution and frequently sweep over the surface
of the IIpccimen to renew the solutioD. When the structure
has been suitably developed, rinse the specimen. either with
a swab 5Iturated with water, or beuer Still. by pouring water.
over the spec:imcn. After rinsin& with bot water, blow the
specimen dry with compressed air. Details of the procedUJ1\
not discu$Sld here are covered iD the sections for the various
metals and their alloys.
7.3 The times given in individual tabulations ate only
intended as guides. In faCt,the prosms of etchm, should be
closely watched aDd etching StOpped when the preferred
strIlcturaJ details have been revealed. Specimens should be
etched to develop structure. Generally, a lialn etch i, bette.r
\baD a heavy etch; overetching can oftea lead to misinte.rpre-
tation. The actual time to develop a structure property may
 r~uv-\j~-l '::1'38 16:10 330 643 9076 P.04
ASTM E34Q ~S II D75'51D DSSSO!~ TT~ ..

4t E 340

TABLE1
AIIOV ~C~
..
~tr8ll"'01 AlUmlnllft'l_ Aluminum ADoyI
CO/llm8Plle
~P'I
AI NeOH 10g ImIMrJe ..,. II tel 15 mln In IIGIuIb! hulAId TOeo Goad ~seeICIIaftt.can be
H~O 1001'1II. 10 70.C 1140 10 1GooF). Aina In witit', IIId UHd on 11/IIo81 .. lllullllnlim 11Io,..
"11\0II9 smllt 111stnIng HNO. I~n. !'IIIIM end 008J nol teQUft ifni G'f/d'IO.
repeat elCHllg If MCH8II'I.

3X1O( HC! (CClICeIftUId) 75ml Mix fnnrh '-In using. UI8 It room tlmpel'lt\lnl. Used I~ cl8vlllop SI'1IIfI81ruc11/fe. May lie
4XJ(X H~(~ (iliff 26 S WllOr 10 IIOw ckrwn
26""- MIl' 118USOd It ImIlltrlllOn "CII or rHIIIIIG dIuIItd 11II1/1
5XXX HF (411II) 5mL aplCimen aurf8ce. RIII88 IpIICIn!8n WIWIIIIIIwater IICNnQ. Does nol ....- fIftt
8XIOC III1d dry. GflndlIICI.
H<ghSicalllnos

HtgII punty A1 HCI (clNllnll'lhId) '1IIII'IIrM IIfIIIC/rnIwtI' fCIDIIII8mp8IJtUr8 unu GetIrId Tuc:kw'II81eh. GIInIII'II puIJIOt8 lldllar
45""-
1XXX HHOa <-nI8O) 15m!. contr.., I&~. AinIe 1/1warm WIll« end MWelnIl ~OfDO\I'Ita&t
3XJCX HF(48 15 /IlL drY. end WIOUQIIt
aIuIninwI\. aoet 110I
010( I' 2S11It..
~O rtlqUlnt tine grI~
SXIOC
IIXXX

AI 8IIC8pt IIIgh 51 Hel (canoantr8ll!d) IS 11I1. SerIte II aIIoVe. 1 .. 2 Tuckw'lI. SIIII8 Ie 8tIIMI. but
CUIInQI HHO.'I (CiOI'ICIIIItrlt8d1 5 III!. IIOW8tdig.
5ml
HF("'" 15 'III..
~O

2XXX HCI(caranllllilld) 1511I1. M8y be UB8IIII M IIII/IIII"ron.1d1 or IIWabbed 0_ F\Iok',....,1. BeatmutlS..

High Cu &lop HF (48 OS) 10ml IN spoel/ll8llllUl'fac.t.WIlen CIaIrod OOIInat 18 Ob\U'I8CIwiIh BvrounclllRtlCo. 1eo
HaC) 9011II. oblUted. tInse In IIIItIf IIIIIIII!IIM .... WdI! 9'11Wfllsullc8.
conc8IIl/'818d HNOa- RInIIe In WI/III WII8r 81\C1*y.

TABLE a MeGnletGh81118 fOl Bef)1IIutft end Beryllium Allor.

"..... Co/IIpotJOoIt ProGocIute 00IIImIrIIB

Be HCI 1011'II. EldI8r f\IIIb or ~ RIOITI...perat\l18 fer . IIW WOIks belt 01\DOarI8gr8ned &e.
I'
NH.CI 40 ninul8&. rinse In \llB1IIr~ city.
H.O 90 mL.

Bo HC! 10 ml. An IlllIIN8i1III wheI'I No.1 does not WOIk. F1ne1Jr8In8CI

NH.CI 29 meI8I
ma"
not toad ,1111I'- ..., CllIi8.
"". '"
PiOIIcI ec:Id 211
H20 so mL.

TABLEa MactHlChanll for CoIIaII CoNlt Alloy,

Mri CompociIlDn PfOCIIIIure CCImIInt8
4tCHBF.V HOI 5011II. Irnll8W specimen In not ICMOn (140 In 180.~ lor GenerIIJ SInIeIUnl.
IiomII Co-Cr 8IIOYI H,O SOmi. 3010 8D /IIln. Alnee In hot water GIld <Sty. poroa1ly.

25Cr-1ON~SW HO 50lllL Sweb until deeIred contrast IIIoll!:Bined #181I nnse In GI8In size. g!lnllnll
HNO, 1DmL
2' Cr-2OM-
3W.a4001Cb Feel,
WIInr WIt8/' and dIy. IUUcIYf4l.
109
".'10 100mL.

CuCb' 2NI1.CI.2H,o 211 As ebovl.

FIC1a 5g
HNo. 5M1.
He! SOmL
HeO 80m

be quite different from the one sugesteC1. 8.1.2 The cold-worked surface should be removed by
machining tbe surf~. Apin sharp tools and cepious
8. Specilk! Preparadon Procedures and Recommeaded Solll- lubrication ate required. If fine deWJ is required, the
acml machined surface should be ground using silicon carbide
8.1 Aluminum: pIper lubricated with water or kerosiDc.
8.1.1 The specimcos can be cut '-'Sins common cuttiltJ 8.1.3 Scvetal of the solutio", used ill macroetchiD& mu:t
tools, hack saws, band saws, shears, abrasive cutoff wheels, vigorously with the metal and can overbea~ the specimen. In
etc. All these mSlhods will cause cold wafk at the surface and these cases tbe specimen is periodically removed from tbe
will &cnuate heat. The temperatu~ rise can be enoush to solution, cooled in running water, and reimmerxd ill the
cause c;baf)SCSin suucture. For \bne IeUOb$ sharp tools and etchan1. This procedure is reptated unul the desired deatee
generous lubrication IlI"CDCC:CSAtY for sectioning. of etching is obtained.

pyri!ht by lhe American Society Far Tesling 4: Materia19

II Bov os 15::15:55 1998
 Ib: 10 330 643 9076 P.05
ASTft E3~O ~5 II Q15'51D 0555D87~32 ..

41 E 340
TABLEof M8cra1lClt8llt8'01 Coppet _ c:tPD8f'AHoy.
r---. AlloY' PRIC8CbB CCrllIlllmIS
C"'"1IOII1Oft
Cu allISIII tIIUIe. HNOa 10mL fmme/'H 8p8C1m1111\
IIISOIUIIOIIItfOCII'II empllasi2t grllnt II'td Ct'ICks.
1\0 IOmL lor I few /IMutH. AI/Is8 ~walllr ""M8
IIrJd dIy.
Cu IIId &1/brU8" "NOs !Oml As 8ba\Ie. BrIngs OUt grIIllI eumrllt, 11I11
60 till unllU 8OitA111C1. "*"t
A/umIr1um brtIna!l
"to
/MY 101I'IIemu! 'IiI'ICtI 081\ be
by bner irrInIr&kItIln
*"'Md
c;ot\QIMrIlect HNOa.

CII 8I1CIII !!rUIn HO 30ml AaIllOve. Goad QItirI r:onlrMt.

F.o. 100
1\0 or 0IIta/I0I 120 mL

Cll.1\IQI\ CllIIIen. K.tCraO, &at 2g lmmenIeI/II8CII7I8Iln solution It rClOl'llllmpel'lllUr' EmphIlSl288 911II11 baund8ll8a and Qj(J1I&
PfIOIPIIon/8. \In IIGIn of HaC! lOt 15 10 3D min then 8W8b wjlh eoIuIIon. fllcjusloM.
tlrPftZBS "aSOa R/n88 In Willi! W81tr 111IIIffy. """
~O
AU HNOot GOmL Immerse speci'nen In adutJon at fOOI'IIternperllllll'l.
~5g RIntt InW8MIWI. .1Id ciy.
HaO 50 mL

StIlt 2O.1OIUD ICIfII 20 mL AaIblMl. SlrD/tO lInee.

5S~Ic:fd 10 till
10 !IIFeC;\,.1rI fiml.
"'0
SIIICorIb'ISf or oronz. Crg, .011 Immw_lJ*!mtnln IiOIUIICn
at room ~.
NH.Q 7.&0 IIIItI wAIII'IWIler and dIy.
HNOa (CGr\GIIIIV8t8d) 50ml '"
~.($uooQo..Ik-.dl 8m1.
~O 100ml

8.1.4 Mat:T()e/chanls!or Aluminum and Aluminum
(Table I).
8.2 lJery/llum:
8.2.1 While: be1yI.lium in the massive form is nOI daD-
serous. bcryt1ium and its compOunds in the finely divided
State are exU"Cmel)' poisoAOUS.
Non; 2-CaIIdoJn Wore JtaJtin& Iny work invoMna beryllium. a
re~ew of llAar<Is And pII,,, tOr hlndlilll mwJcI be made. A number of
roll:renc:cs 011 beryUium an: avail8ble. Plnic:1IJar menlion
I)( "ToJieity of BeryDium~ ASD-TR-62-7.667. prepared by the
.KetttriJlglaboralOrY for the Air Force.
8.2.1.1 Generally spea1cin&beJylJium and its aUoyshave
given difficulty in obtainiDi scod macroc:tched specimens.
First, bctyllium is a rather brittle metal and sectiOniDScan be
difficult. Cut-olfwbeels with the desipation C46FR70 have
~n the most successful. Secondly, bayllium does not &rind
easily: bence. specimens should be as smaJl as possible to
minimize pdiDS time. Grindins has been most successful
with tbe entire sequence of wet silicon carbide papers.
8.2.1.2 The: etchins affine grained metal may not always
be enLi.n:1ysuccessful, and further ~tion will be re-
quited. Rouch polishing with 15 pm AbO] suspended in
water is performed on a low-nap cloth. 1J&bt pressure and
frequent cbange of euUine direction produce the best results.
If further polishin~is required, l-JLm 81'CCllCr20! in tap
water On synthetic suede worb bcn.
8.2.2 MacTOetchOlfts/or 8ef)'llium IUId Beryllium A/loy~'
(Table 2).
8.3 Cobah and Cobalr Alloys:
8.3.1 Maay of the cobalt.base high-temperature alloys can
be etcI\ed UUIII the same procedures as those ror iron- and
nickel-basc high-tempenuure alloys. Other cobalt alJoys,
Alloys such as the stcllites used u machine tools, require special
tICatment.
8.3.1.1 The cobalt.base alloys. as a grouP. are not easily
machisaeG. The specimens $bouJd be sectioned with abmive
cutoff wheels and ground on wet liJiean carbide papers.
Because of the rapid wort-harden:ing d1aracterisdcs of tbcsc
alJoys, fic:sb pallC'fand copious QOQJinS$hOuid be used.
8.3.2 Mae'Ot!lchanlS!~ CobG/t and Cobalt Alloys (Table
3).
may b~ imide 8.4 Copper and Copptr AJloys:
8.4.1 These: metals are usually macroetcbed to brins out
the leaeral stNctUre of wire bar and billets as well as
variations in snain size in eJt\n&Sionsand forgiolfj.
8.4.1.1 Sf)Ccimens may be sectioned usins common cut-
tins tools. To minimize cold working the tools should be
kept shal]).
8.4.1.2 Good results can be obtained by machining a
smooth surface in two maca, the fust beiDi a heavy cUt to
remove the cold work from sectioq and the second a fine
cut with a V.shaped. tool to remove the remainins coJd work.
Grinding through the series or metallographic papers will
give more detailed results. The degree of grinding depends
upon the amount of detail required. The etchiDi $O\utions
listed in Table 4 are simple to ptepan: and their use requires
no special technique.
NOTE3-lt mOllld be:J)Ointedaut WI heavy achill' aften win
fCmo~ the:cIT~ o(tol4 work but at the eapenx ofproesucillli rougb.
surfDce.If the &)IeCiftlenis dIeft plteD li,cbt rql'illdilll to remove the
roU8h etchecl CIIIf'.cc, the seeond eceb wiD provids &oocf resullS.
8.4.2 Macroetchants/or Coppe, tllld Copper Alloys (Table
4).
8.S 1'011 tlIId Steel:
8.S.1 Macroetching bi15been most nighty developed and

)pyright by tJ1e Ameriean Society For Testing a: ),f/lCenBIs

~ Nof' 05 25:98:05 1S19l1
 I ~UV-IQ;:>- ~::1::1t1 lb: 11

AST" E3'1D Cl5 . U'/~'1~.LU

U.:5:!:luauUt . _ 330 643 9076 P.06

eE340
~TAIIJi & MaarD8W1I8Id8'ar Ind .....
AIDyt '"'"
COmpa8ifcn ~CaIIIm",ta
PIIIn IlWlIIIOy..... HCI~ SOmL tmm_ In toI\IIIaIIlI8aI8d CO180 to 011I8I'11 ~.
.9'--"
h/QIMIP88d 8IId 1oOI ...'" ".0
&GmL 'SO"F lor 1$ 10 30 mfn. DeemuI by vIgcHous
CUIIIy (12-14. CtlMCI fCI'\IbCIrIg ........ ... bIIIlh U/MI8'
Wi'"
a18/nIIII I\IftIWIg wMIII'. StI/nIeIs II8eI8 mar be
."'" cIe&mIA1ed by _119 In I Welm 20 S ~III
giv8 I brtghIlIIi8h.

HIgIH\IO)' .... HCI (COM8IIIrII8d) 150mL Imm8IIIepec8ftInlar '0 to 15 milliI ~II RallO HCtHNO. runs 2:1 3: 1.
HNC,(awennf8cl) 25mL r~ ~.RIn8eIn.,,1IIII1
\IfItIIrend '"
2SmL «,.
PIIIIn8M
... _ steels. CUIIIIY
H.o
HCI (CXInI:BIIV11ed)
~SO.~
3BmL
,21111.
~&pBCl/Mll1or 15 45 tn1n In lIIIutm
IIoIttOIO 110 10 1&O'F.'"Rileelllw.m"'"
work8 WIllon
'2 . (:r 11881.
HaO 5Om\,. II'ICJIlly.
HjgIHIIoy ... HNO. (com:8ftlfllted) 10/11I. IPIIm8N specimen III8dutIon hlltIII 10 160 10 Ral!o H~HF varl...
HF (4' !II '/IlL UlC"F urdUCIIIIrvdItch 0btIIn8d trill mil
81rnL In WIIJnw&tef end drY. "
"*0 8111II.
KaC
10
HND. (COIICMlraW) 40mL
HF (4' !II 10/11I.
HaO 50mL
SIaHtts a1ll8ls.IIIg/IoIllOy HCI (CGN'8ItrlJled) 150mL MI. HCIand water 111Mheal 10 180 10 '?O'F. Produces DIIgIIIIUIIsII.
..11 HaC 1iO/III. Immene epeaImen 11IIII_ HaOa In eevtrll
H2O. (all S) 20mL pw. 011 I'IGImtL MIle, 88Ct11U11t8Q111ft1
8ddI8oII .,.., foImIng 110m tnVlOuS eddIIiOft
ltoppICI.
SOmL
""
Au8t1lllliO ItIIIMIn 118818 He! (ocIftC8ftIr811c1)88' ImI'/IIIft IIpIICInIen in ICI/ubCInIMw:h rI\IV lit MnIe'& reqent. ~Md!.good fur
soIn
CuSO. In H,O 25mL
IIUI8d or nol d8JIIf\IIIIIa upan 1Ioy. TIIII8 ....
dlOll'dt Oft~. Rlnleln wann W8ttr end drY.
.~-
PI8Inandlcw-8IOy ..... (Nti.IaSA (8mmo- 10; Swab tOIIItIonat room 1lmplfl1Uf. tNer Gtlln 1iH, wOICImtrIt8.
III\IrnperNf8llJ JOICiIMn, RIll.. 8M ~.
HaO 10011II.
PlaIn8IId Moy atellt Cue!. 2.Sg 1mn181!11nIllMion at roam tI/IIPII'ItUI8 unIII8 SI88d'. ,..,,1. S8Its d\UOIV8dIn
M&CIa 10 II COJIPIIYIIhIIn IIfIp8IF&.Flln8811\OrOUC1111YIIId HC1with DtIICIIwider. To
,,-.... HCI(1ZIo_.1l1Ibd) 5mC.. dry. bring aut "'"""""
Pofttl BnIU IIIIdP
A~IO 2IiOi'lL liunGln9.
MIldlSteel,e-Iftd high Cue" 900 'The surtace I1'IoUId be I\IDbed willi cIolh II08ked Fry'. nragom.. Befort etc:hInQ,'ample
~11881 HCI(WIf*I-1IIb<Q 120 mI. In ~101\11101\.
WIfi/I In IfoohOIOf r1neeIn wu!d be h8a1ed 10 2DO10 ~C
HRO 100 mL Hel""") aller etehll1lllO prev8llt 08jI0IIII0n 0/ (302 104I2'F) lot 5 ,., 30 /IIIn
QOA8f. d8p8rICIIrIg
an Wldlilan gf .teet. TO
ahow IIfIIn al dullO caleSwork.
PlelrlIIIId IIIoy Item CuCb 4511 AI 1bcMt. ModIIed Fry'. I'8IQeIII.S8rneasfor
HQ(~ 180mL rIIIgItIf foiO.9 IIUtmoIIlleCllIy
HAO 'OO"'~
Wazau. maygMI_ canlrB&l
8JIfIIGIIIIn
CII\ 118W88h8d In waler
.",1hDU1dIpO!iIIIr1g ccpper.

SI8Ir\IIS. and I\IgIIoCr&t88II HCI 10rm. llllme";8 IIp8dm8l\ 1ft8duIIOn at ~VII88I's f'llllllII1t.
AICOIIcI '00 mL temp8fllt\lr1 until d8llred ccnttw Is CJbt8Ir\9d.
PIcric ICIcI 1 II FIIn8t 8nd dry.

PleIn and 8IIDy .1eIIa HCI (canClllvatacll 610 12 i'lL EIIchIytIo. Ii to 111A per 8Q\I1II'OIIIGII.apKim81 Smell sps.imltlJ. <20 III.a _
H2O 100 mI.. ver1lal. rInae. brulII. and fly.

Plain and lIIOy .... HCI (CCR8r\trated) 8ml !IKIroIrtIc:. apeOlml/l mov.. ~I. c:atllaae tier. FOI spsdIr1ena 0V8I' 20 11\.11 8f88.
~,00mL. 30 tD 40 A per 1nd1 o1l1p8C1men 0MdI1I.rIMe. t)jooma, 1ItIIeI1. and llebl.
Hea. 111 bruIII, IIIId dry.

i.gused eXtensively in the iron and steel industries, In Mt.mill
products sueb as bars, billets, eecr, and plate, the disk cut
with a parU11&1001 is prepared by facias on a lathe or by
grinding. In facing. the first cut is modm1ely heavy with a
sharp tool. The 5eC01'Id.facing is a light out with a V-liMped
tool run at hiBb speed. SpecimCIIs produced in this manner
are adequate for general i~ft. A better mouCh slower
metbod is to grind the specimen. For inspection purposes,
finisbm& on a 12Q.grit whee1 will be sufficient. If machine
grindias is used. the specimen should be of a size that can be
held conveniently in ODehuc!. The limiting size in machine
srilUl.i.oais usu.a1Iy12 in.:l (305 mm~) sinoe 1ar&etspecimeos
are difticult10 handle in the etching. bath.
8.5.1.1 When the maxim~m amount of detail is required,
115in weldmeJSu. poJishin,e the specimen with the series or
metallographic papers gives tbe best results. Wben exam.

Copvn!ht by lhe American Society For Testint IfMBferials

Thu Nov D5 15;38;15 1998
 __ 330 643 9076 P.07
AST" £340 ~~ .. U/~~~~u u ,w, . .,'

OE340
TAILE' Macnl81CNnta'or Stelftltll SI8eIslIftII "gII.TlntpIIIdUte ADap
AI/QyI CG/rIpaIIdIiCln Pn:adlll'l COImI8nII
St8/IIII8a __ IItICIIrvn-IIUe tfCI ~ 50 lilt. IIN'nern IIJIIIdMtnIn IOIUItonIIIId8d 10 180 10 GIIIerIIIpUfpDl8.
~1Ur. .,. 180°F lor 30 fIIIn.DPrnui Df vIgoI'oUli
8Q'~ with Vt98IIbIe bMlllIIIIIIr runfting
watBI. _11I888 .I.1181!11y118Glll/NltIIG Dy
~ppInv III warm 2G HNO" tel give Dnght
llI1IGh, "

Ir~. GObIII', , ruck8Hleae HClI~-'tdI SemI. !nvMra8 8pICIIII8II1'I101u1lon 811'1IOIII Rotio HC! + HNO" "",I 2 or 1 10
1IIgh aDo,. HNOa ICOI'DnIrIIIdI 25 mt. lemperalul1l tot
'0
10 SO min. RInSe IIICI dry. 3 +,
~2511I1.
StaIn_ 11II8II ,.nd tI'fO~ lOmt. '",,*18 speamen UlIIOIuIIDII llBII* ID 1IG 10
/llgll-181'/1pe1'11\1"8.. HI' (48 !I) S/IIL. 1SO" UIIIiCllWed ccntrest II obi..,. Ami
HaC 8rmL 11/IIIIlly.
1O
HNOs (GOnC8\!r8I8dI .tOml.
HI' (48 15) 'II /IlL
HaP 50 mL

Au8 ~ II8InIea Sleetsand I (......!JSO. 15s CoInbJn8 I Ind IIIhsn 81M m. ImlNl68 8P8f*n8n LepilO', Bleh. I, 1IIIII1r88h. grain
IIIGkel b88I ellaYa 75111L In tDIutIon roamlelllperiture umiI de.., IIr\.IChn.
"'0
1\ FtCJ; I'
2509 cOnt'NtI8 OIIIaIned.
t4C1(c:oncenIratlllJ) 1DOmL
III HNO:t 80mL
(CCWICMIfIt8d)

AuBlIri1IO 1181.-. .1818 IIftCI Hel (conctrI1ra11lCS) 50IIIL MiltHClInG WIII8r hell, -1fI8CIIr8n
~I\n 8iIOf' HaP SOmL II1dadd HzOI "*'88V\11'11
pII\8, 00 not..
HaC. (30 S) 20 mL Mllee e8CII~ " IddI\IoIIaft8r fo8mIng
/rom jjftlllawll4C!ft/an ilia trappIid.

Au8I81II1G IteImIl InO HCI {COIICIII'ItrII8CI} 5011'I\.. IlMIerllll cpec1/rI8IIl III sDlUUClnwlliCll may 08 MI/tIIe', ftIGIIIL I.JOIItelCh. lor
""'I 8*
~an eIoya Sat IGIngf 25m/.. heal8d up ID 1100F unl. dllllll8d contrut 18 &In.aI.rll. AIIIOUIIt01 CuSO.
, dry.
CIISO. IIIH:aO cbIIIned. RInoe 8OIIdIDII1IIIIY08 iKnaI8CI to 1 ... 1
'1110 far /lllllQj1t .1.

TAILE 1 MHr..hant8 for Lll8Clllld Lead AlloY.

,.., CaIIIpOII1IDn p~
I..8IId II'ICIIMd 250 PIlL AliI!A to 8 INlIeI praaIpItal8~,. If8 II lidded10A II"
IIfop 140/ill InIOIUIIIe pr8dpI\IIIIformt.
110mL AddC 10mIXUItat AII1dB IIfI8rpnIdpitIIeItaanedlUoMld.
1DOnIL.
9110mL &weD SIl'fIlC8 oIlt18l1p8dm1n with mIqd 8011111011unIII 0III1red
'DOnIL. conhIt 18 obIBInttd. RINe 8IId dry.
100 /ill
AnIImoIIIaIINII A. GlIOIIIII:ItI; IIGIct 30mL ,., IIIMftoeon 8ik v t wIIeeIwilt! AlA IIbt8IIve 81 150
HN(q {caNIIIIht1ldJ 4Dmt. rpm. EId'I wt118IIIU!IDnA II,,"C IIIIn , 11I11I
tJr¥L
HoC 1SmL AIIfCII wItI Elil 1'1IOIII
tem__ fef 1 to 2 h.
8. Gl8ClIlIe8IIC IICIIf 1 mL.
..,0 4DOmL

A. HNOa(~HJ 8DmL M!1I1qU1I qlll!l 01 A IIIcI G 1rnIII8dI,IIIIy IIIhq I/IIm8f'e8

HaO 220 mL IjI8CimInInsalullan11101IIII
~ "'..
___I
B. (NHo~O. 45; Ie cbtl/ned. RlllSlIIICIIII'y,
HaO

A. (NH.>.MoO. log I/llIIIenID epodIrIIIn In 0GIuIiIIn .If _ IImperabll'll \InIII deeiNd Stlgru e1\1I. !lIEn
Q1IICIdS 25 . contralllB obIIined. Ih8n tl'lllll1IIIII dry. IVUctln. CIIf8cIa.
HaO 100 mL
A. /\aide: IICiCt 75rnl. MIx with 8\IOngIII1 HA IIVIIIItIit 1DmniIIIz\I WIIIIf CIQIIIInt.
HA 25mL IrIVIIIIM dry 8jI801m1n 11\*AIon IlIIICIft lemDftlln
""III
~ c:anIIIIIt18obIIllIId. IinII dry..
"'

iniDa for 5W'fiM;edefects, the surface itself should be etched the sIJrCac:euJldcrncath. If care bas been exercised in the
dirtetly without much preparation, The only preparation grinding operations. the gritsding 5CJ8tehes will not intufere
that is advisable is to brush ofT me loose scale and then \0 with examination.
give the specimen a light grinding pass with very coarse 8.5.1.2 The most commonly used solutions for macro-
abrasive to break 'lhrousb the adherent scale. When etching ctchin. iron and Steel are Solution Nos. ) and 3 in Table 5.
in 1 1 HC1 for exampl.e.,this scate will be R!moved. e.xposi11.& 8.5.1.3 An electrolytic procedure u$ing 6 to 12 % HCI in

CoprrilhL by Lhe AmeriCII.D. Society For Test1iJi IE Katerials

Thu Nov D5 15:38:23 1998
 lb: 12
330 643 9076 P.D8
ASTM E3~D ~S II D?5~S10 U~~~U~U ~~f ..

o E 340
TABL£ 8 MactOetall '01 M8I"Hlum IIftd M8;1III81um Moya
Alloy cQflll108lban ~ CO/MI8I1I8
ZKlDA GIICIII tceIIC IICIcI 5 mL 1/IIII'Itr88&p8dmon ~ ealulkln at IIICI/II Flaw IIneIm fOrOInI..
H,O alIA lor VII10 8 mm until f88Ir8d CCIIftIt Is
85mL 00tIhId. D8IftIIt wfth &0" HI' ,..II) In
MW. A_tn qpIdIy IIOWIIIg WI!*' ancI
dry.

AZI1A Glel:lalIIOIUO IDd 101M. N IIIIav8out for ~ /0 5 ft\II\.

AZ8DA H~ eOmL
AZ3'B Glec:l1I 8CeIiC 8dd 20m!. As IIbov8 but fOr \Q to 5 11'I1/1. i=lOw PlIIIIr/lIII 100QIIIgL S\llf8ClCUuna defec:1J.
GI\'COIICKId "lIlY be BUba1lMld 101' _III: add.
AZG1A HaNOa 5\1
AZ80A ~O BOm!.

AZ318 HNo. Iccncentr8l4dl 10ll'lL ,.. above ~I fer ~ 10 5 min. Raw paalm In 10r;/"g8. IrIIOM8I~ IIIcatl
HaO go III\.. IIIaDIll'ld IrI;oI8.

N8aO',O, 180g A&IIIIove bur rI!II8/n hot water. GIllIn Met!for cIef8c;1s un.. IIIIddie I8SUngs.
HNOa (wlCIeIlWIIUIdl 180m!.
HaO to IIIIIIc8 1011O!IlL

Cra. 280 iii OeImInBllonon IMd CUt 811t11c8s.~

HNOe (coranII'I*'I 2511II- aeletts 01 die cestinp.
HF C.a ') 'OIl'lL
HtO fa mike 1000 IIIl

AD1A 8 S pletle Belli 1ft IIIOO/ICI tOOIl'lL Aa BOO'" lor V. 10 a m/n er "lIlY be 1WIbbed. GreIn 81m and no. P4If8n8
0'
botII Clst 8I'ICI
W!ou;ht formt. Aequns fins /Hoh (500 grI1I.
ADDA H:IO 10 mt.
G1IOII ac:eIlr:BCd 611II.

AU' e s pIc;rIc IICIcIin llCOIIOI 7011'1L AaNo.7. GnIIneIIa. ~ ¥ho\M 1:18fhshed an

6OO-trft peper.
AZ31 H,o '0 IIIl.
GIICi8I K8IIc acId 10mL

8 S pIcIfc:fIdeSIn IIIcahaI 5011I1.. AS No.7. Flow I)IIItem INI gf8in II. 01 homoglll18OUS
HaC) 20m\. BIIoV.Incr "'181' to N8111S 1111/1I
eteeI8I _~ ICId 2011II. GOnIr18l s,**,*" .atIOIMIbe ,,",!hid gn
800iIfIt PIPIr.

.. picric 8CiOIn IIIcahaI 10011II. Imm8rI8 speclmllllin 80IUIian ac IDOI'/I SIgnIQIIICIn olln\8llftet8IIC campounds II'Id
HsPO.
" O.1I1'1L lemperallA ltP08IecIy until dBJIJtd ota1n III ar0d8I.~. ~ ~0UId be fInl8/I8d
~lntIdo rinse 11'I11II/)'. 011~t )11I$8'.

water at room temperature may be used instead or hot I: I
HCI in water. This proeedure reduces the amount of acid
used and minimizes me ftames usoeiat.cd with hot acid
SOlutioDS.
8.S,2 Fo1'gings-1D addition 10 the eumioatjon for in-
ternal structure. surface defects., and structure, cloaed-die
Corsings are often UClioned to show now lines. Etc:hins for
lIow lines requires extmneIy careful preparalion to provide a
smooth surface with a miDimum of cold work. Lone
piecessuch as crank shafts arc awkward to handle and an:
best prepared on a griudiUS machine usins suc:c:essivelyfiner
IrindiDg wheels. Sectionin& into shorter leD8fhs may be
advisable. The ~men shouJd be beavily etched in 1+ I
HC or 20" H25O.. ContraSt caD often be irn;reased by
wipingthe surfacelightlywith very fine me1a1lograpbicpaper
after etchinB- ExamiDa1ion for str\1Cture,defects. etc. is
carried out in the same fashion as hotmill products.
8.S.3 Special TestsJOT~ion- There are a number
of etd1an1scontaining copper salts which will reveal segcga.
bOn. Careful specimen preparation tbrougb the m;tallo-
paphic pa.,ers is requited. Very careft11cleaning after &rind-
ing is extremely important. When a specimen is immersed in
this type of solution. copper plates OUtonto the specimen by
a replacement reaCtion. The rate of deposition depends on
the composition oCthe steel and the copper plating will cover
the segregated regions. Sometimes the specimen can be left
in a littlc lonaer than recommended and then rubbed lightly
witb metallograpbic papers to in<:mue contrast.
8.5.4 MQ&ffJt!tchtmJ$ for lr01l and Steel (Table S).
8.6 Stai..ms Stms and High-Tempe1tJlIue A.lloys:
8.6.1 These alloys are geJltraily more swccptibl~ 10 cold
working of the surface than are the lower alloy grades of
steel. The best method of prcparaUon is to grind the
specimens as described for iron and steel. A smUt tends to
form on the surface of the steel when immelXd in I + J MCt.
This can be prevented by adelia. a small quaatity of HNO)
to the etching bath. It can I1so be removed by sc;rubbina the
sPecimen with a vegetable fiber brush under running warm
water or by immersioD in warm 20 55HNO). Scrubbing will
ptOvide a bieber contrast for detection of searegatjon and
inclusions. The desmuUili1 either by Ihe addition of HN~
to the etCbing barb or by the secondary rinse in HNO, will
provide a brighter surface which is suitable for determination
of grain size and &uuCture..Hi&b-alloy stainless steels and

CopyrlgJit by the 4merican Society For TesUDg KGt.erial!

DIu NDf D5 15:36:30 1998 '"
 Ib: 1,5

AST" E3~U ~~ .. W..OfI#-"._ _.. 330 643 9076 P.09

.
Ut~~~~u

E340
TABLE 8 MeCf'Cl81Chllnta for NIckel Ind Nickel Allor.
Oompoajllm Procedure CCII1IIIIeftts

HI OIlSO. IDe Inun8I'81 IIfIICImen IOIu1Ianat _ WI\pInI' MaIDIe's I'1IgCIm, lor IlraIII wuet.vre.
HCI 5OmL. 11ft unlll ,'" COIIUut Is obteNd Aillall
",0 50mL and dry.
aOmL Imrnena ep1Q1'1811 In 8oMion II rGOIII 1Bl'llperJ- GraIn sllUclure.
10 ml. IUI'IIfor 20 to 30 MIn, rlnsland dry.
10 II

~ 50mL Immerse &pIIiIm8I In hot -.oUlon. RInse In hDI GrI'" struc;Me.

Ao8te 8c:Id SOmL weier and dry.

ACI~ adCI SOmL SwIll Leplta', reagan! U. etl:ll8nl fill' nlcl<eI

H/IIOa iOmL WOIIJ8.

Sit I!IC!!n01 CuSO. 50mL

In H,O
He! 50mL

Het 100 mL see 405.4

HaC 100mL
H:.O. (30 S) 40mL

TABU 11 MKl'OIItChantilor thl Noble MM818

Metal CCIInpQ~ of Solution COI\dItICn of VIe Convnents IIId Use
Ag HNO~ 10ml.. FIT. taw mmut.. Gram OCInlrUI.
Matllyl lIIcDhal BOmL

All MOl 66mL Hell, mlIIUII.. Grllln contnIll.

~PIatIoya HN~ 34mL '"'
Pd...
Ru IInd BIIDyI LAcUC
add 50ml RT. few l\'IIIIUIe&. 01'1II'Ic:onIresl.
08 IIIId IIIoys MNOs iOmL
Rh 8/lCl1IIIr:Ip HF SOmL

All ebCIIte HCI ~mI.. AT. f8w IftIIMn. O,aIn c;g'\trll&l.

HNO, 15mL
MF 30mL

I't ancI 8IIoy. Sat IC11II1IOn01 8C>II\L. EI8CIJOIy!Ie, 5V, 1_ GrBln C4ntrallt,
NaCi III HaO 1oIIeI. ""n-
HCI 20rnl.

TAlL.£ 11 Macrwtcll8nta for A.,l8C1ory MIC8I,

Metal COmpc8IDonof SoIuIIon Temp8111UAI -nm.
Mo,W, V, ~, -.t Ta HCI(canctII1I'1II8d) 30 AT 5 1020 mill
~(concMlftIl8d) 15
HF (48 I) 30

Mo, W, IIIId V HF (49 S) 15 RT 10 1020 mln

HNO:a(concanllltet!) 3$
HaO 75

W. V, CO, II1d TI HF (48 ~) 10 FIT , 1040 Too 'ast for Mo. , 10 5 s

~(CCnc:8nIIItGd) SO '"'"
LactIUC!G (115SI 50
Or H"SO. 10 BokIa 2 105 ,"In
H:tO 90

Copyright by the American Society For Testing ~ Klterials

Thu Rov 05 15:56:38 11198
 330 643 9076
U...,.,\,I..._..

GE340
TABLE 12 Macroelchaft\ far Tilt .ft. TIA AI\o18
~ 01 SOIUIIon Pl'OCBdute CornIMnl'
5al1RIIDCI8n1mOIIIIm poIyBuIlIde Immera ~ .un ItIWlQUI
ooIutIOI'I
alroom ~ for20 to 30 min.Do!lOt.web MIICt GPIII/Iwuetll"
cIurIngeIeI*Ig. "

TABLE 1& MHraetch8ltt. lor TItaniUm, ZlroonlUm. HtfnlulII and TIIeIr Alloy,
NI.Dr ~ ~ Procedure CommenIa
11~1 HCI(CanMIItraIIdI 20 mL. lmmer.Ie specimerI iI'I ooIuUoI'I healed III 120 DeImUt 1'1,-1av." CNlA1, 8110\I0.OIlWa
(q $1 44 mL. 1111~.I' lor 20 10 3D1Nt, Aifts8.II ""lit do lID!notmIII~ ~ ClllmuIWlg.
"F
H;O fcrmeInIrneneInDO$ ~. lOr3 fIIIII.
Rill" IA4 Gry.

7A1-'Mo HNO, (COIIc:efIIraIed) 42mL As 11I0118.

*'"
HI' I" S) 8~
Ha° 50mL
%t, HI, IVId lOW ~Ma~ (SO S) "Gmt. Swab IpIICimIrIwiVllOhdlClnat fOOftI SIIaUId III UI8CIuM8t IIIOOCI; CllIIIIICII
HNOo ~Ied) 45mL lllmplllilhn. AIMe 1D 8 BIteryellowfumes poIIs/jng lioluUon.
HF (q $) 10mL farm. 1I1endIy.

Zr, HI. and high IIIIC¥I litO 45mL As 8bo1I8. M lIIove.

"NOs 4Sml
HF 10 mI.

1.5Sn.o.15F&-O.1OCr, HaC 70 /IlL Aa atIa1I8. As IIIIove.

aM HI ~ICOIlC.on&odeO) 30mL
HF(4"") 5/11L

lodele TI MaCa (30 $) IIOmI.. Swab wIm sDlutJon at room lcrnper8tuIW until As abIM.
";0 3011I\. cI08Il11dCOI'IIr88t f8 dItIIned. Rlnae In eeld
~(4U) 10mL wsw IIId ory.

tABU! 14 Macroetch8n18 rOt Zino and aw: AIIop

AID)' ScI\AIOII
CMlpcelbCII Proced\II'e . COIMIIfttl
Cu..frlle _ 8IOy& HCI(CO/IOII\1rt.ItCII &0mL ~ ftJIuIlcIIfOr 111CU11 &eec:.
II!1118118 ~ 8IPUCfUI\t.
tftO 50/ilL ~.. II,IIWfPng
underM'I'IIng
WIlei'.
*-'
A8MaI un1II delllIO OOftttut It
0I:ItIIIMCt.!hen dIy.

OrO. 200 IfnIM'ee ., IIOIuIiCII UIItII gocd convulll

Nl,;SO. 1.58 cbIIIned.RIM' InI"\IIftng,,111II"
~ dry.
0' Repeat . lI8OIIIery.
Na~",'OH..D 3.40
t\O 100IIIl

austeDitic biBb.temperature alloys because of their extreme
corrosion resistance ot\en will give trOuble in ctcbiDg. Aqua
rcsia, HO-H102> and Marble's reagent are the recom-
mended etcbants. AU three of tbese require very careful
specimen pxeparation.
8.6.2 Macroelchanu for St/li11!essStel!ls and HiglrTem-
pertllure A.lloys (Table 6).
8.7 Lead ad Lead Alloys:
8.7.1 Lead and its alloys are among the most difficult
metaIJ to prepare for macroctchiJJl. They are not only very
soft ud cold work wily, but they (pure lead especiaUy)
recIYstaIJi%ereadily at 1empcratures which caD be easily
achieved in carelC&$preparauoa.
8.7.2 For best results iu the macroetching of lead, all
surfhees other tban that to be eumiued must be masked
from the macroetc:h by the use of several coati of a plastic
spnay. The sun1U:e 10 be examined should be tiled prior to
etching.. Three 14.iD. (360-mm) tilC$J are usually required
)
IoIIcblllioll dCIi.-uona. lie IIIR ID pn:scrw
","",," andh-..anbhilll ._h.
and wed in the following order. (J) aluminum, Type A, (2)
band 5mooU\, and (J) baod-fiuishiag smooth.
8.7.3 The faleis usuany held in a fixture and the specimen
is drawn over the me proceediDe from tbe point or the tile to
the tang. Remove the mings after each pass of tbe specimen
with a few short strokes of a brass file brush in th~ direction
of the last CV~oftbe 61e. The mOlybdate etch listed in Table
1 is wed in the removal of worked metal and aJso to reveal
the auucturc of lead oflow-aUoy content. The preparation or
the solution is of paramount importance.
8.7.4 MacroetcltanuloT Lead and Lead Alloys (Table 7).
8.8 Magnesium:
8.8.1 Features detected by macroe~inr; are grain size,
segregation of iDtermetallic: compounds, coring, c~c:ks, po-
rosity, laps. genni.natio05, surface bumins. and tears.
8.8.2 Cast or wrought magnesium alloys ate prepared in a
similar manner to aluminum or copper and brass; however,
a fina! faeiDiwith a O.OOS-ia. (0. I27.mm) nldius V-shaped
tool (ed at a rete 0(Q.002 10 0.003 in. (0.508 to 0.762 mm.) is
die dinillc:lion belWccn hllAd oiteD suft"lCient.For some applications, the sPecimen may be
finishedon a 400-grit wet wbee1.To resolve smaJl detail,
9

Copyrigbt by Ihe American Society roc Testing II Matorlab

Thu Nov 05 15:36:45 1998
 .1.0-14
M.a,.. ~ "
additional polishing with a water suspension
Alundum or further with alpha alumina may be necessary.
8.8.3 The finely divided masoesium as chips or swan is
hiahlY combustible and precautions againSt it catcblng tire
should be takeo.
8.8.4 MaC'foelchtmIJ for Mapesium and Mtl/Pfesium Al-
loys (Table 8).
8.9 Niek6llU1d NIckel .4J/oys:
8.9.1 Niekel alloys cold work easily and their preparation
is not always easy. Grinding produces the best specimens.
Low-nic:keI and cobalt alloys or basically pure metal. can be
etched with Marble's rcage1\t or strong HN~ solutions. The
bigb-temperat\lfe alloys arc diftiwlt to etch. F"arstof an. they
an subject to cold-warkins problems. and secondly, tht
alloys are extremely corrosion resistant. Bcst rcsu11Shave
been obtained witI! aqua regia, modified Marble's reagent, or
HCI-H2~ soJutions.
8.9.2 MacroetchJlnlJ for Hiclcel and Nlclul Alloys (Table
9).
8.10 Noble MelaJs-Ag, Au. Ru. Rh. Pd, Os. /r, and Pi:
8.10.1 These metals, in acnetal, are soft and ductile.
Because of their expense, usually specimens for macro-
etching will be small and can be handled the sante as micro-
specimens. Care should be used to avoid cold work. Well.
lubricated metallopaphic papm are ftconunenGed. Some ot
the platinum group metals, notably osmium an.d rhodium,
arc more abrasion re&islanl thliD \heir hardness would
illdica~ and, therefore, will require long IriDding time.
8.10.1.1 Exceptforsilver,aUof\bese me1.a1s are corrosion
mistant and l"CQuitethe use of strong etcban1S. Btchinc
should be done under a fume hood, with the proper
precauuons for the use of Uf.
8.10.2 MacrtH!tChfJ1lU!orlhe Noble Metals (Table 10).
8.11 P4'rtJClory MetlZls-Cr. Mo, JY. V. Ch. and Ta:
8.11.1 The above six metaJs, tbe reftacCOry metals, are
found in Group V.B (V, Cb, Ta) and Group Vt-B (Cr, Mo,
W) of the :periodic table. (Some tabJes list them as V-A and
VI-A.) Jo general, tbese metals are soft and ducdJe in the
pure state. but iD the Conn IISWIIlyencountered arc hard ud
britde. Consequently, thcac metals and their alloys must be
carefully p'ouod before macroetChing. The abrasives mUStbe
of sufficient hardness, and. particles 011 the laps must be
sbarp. Wet silicon carbide papers have proved Atisfactory
provided they arc used witb sufficient pressure to effectively
cue the sample and are nen wed after they become dull or
wom. Lonacr grineSina nmlS than would be expecced trom
&behardness of these metals and alloys are needed. The
solutions listed in Table 11 used for the metals speQfied will
reveal dcfeecs. genen! struc1Ure, Bfa,n size, and sectClltion.
8.11.2 MtlaO(!lchants lor the Refractory MeIIIls (Table
It).
8.12 Tin and Tin Afluys:
TMAmtllt:/ln ~, IfJ'TIIII/I!g II1Id """",1II/81811U /10 PGf/f1Oll ~rIf1lh8lf811d4y
WtIfhlIlIYJ/MI mMlictlH 111ItrJa SIMrMtrI. LlalII 01_
paleIJIl'fgIIU, IffJd UIt llak DlI1/II~ 01 6Ur:h '/(INII. .,. 8f'Il11'elYfNIi' own rppt1tQ1bl1IIy.
1'11II8I1f1de1rJ ;, .., 10 t8V18/atr II! IIIJ' IIIIIt
.. WIIMtI\IIrL YDIIf_8IItI81'8
"ftfIf ,..."..,. tIfIrIff 'tI/PPI'O"
end IItGuId ~ IV A:mrI HfIII6~.
I8IIhtI1MJ C8MJ888. WIIICb1011 ~ 1IIf8nG. /I ".,
'"
"18WIrtnOW/lIOme ASTM CornmIIme con ~.
Copyrlghl by the American Society For TutiJIg ok Materials
Thu Bov 05 15;36:53 1998
3313 643 91376
e E340
of 600 8. t 2.1 Tin aDd its alloys, li'k~lead, are difficult to prepali:"
Because these mews cold work easily and recrystallize LJt
room temperature. faise S1n&C\U1'eS are easily produced. The
belt method of preparation tor macroCtChing is the same a~
(or microetchi.n8. Tha specimen should be cut caref\1l1yand
them.around gently on lubricated silicon carbide paper. Thi!>
may be followed by polishing with 6.Jin1 diamond paste on ;,1
moderately nappy wheel.
8.12.2 Precision cast tha-bale beariDi alloys may be
etched directly without preparation.
8.12.3 Ma&roeIchIUIljor Till and Tin Allo)ls (Table 12).
8. 12.4 Prepo.raslon of Ammonium Polysulflde-Pass HzS
gas into 200 mL of N~OH (sp gr 0.9) until saturated. The
solution should be kept in 110ice bath durinJ this operation
Add u addiuona1200 mL of NH.OH (sp g,r 0.9) aDd diime
with watertO make 1 L. Add 100 gofsulfur. StiroccasionaJ!y
o"er a period of I h, then (dter and use.
8.l3 Titanium, Zirctmium. Hqfnium and Their Alloys.
8.13.1 Titanium, zircoDium, and hafnium, the reactive
metals, are maaoetcbed for &eneral structUre, pin size. and
aqrcption orimpurities. They reqwre eXtreme care in prep~
amioo. Sharp toOl8 ud fresh grinding PiI'Cr' are required to
pn:vcnt cold work froID blurring the structUre. The best
results an: obtained by &riDding. These metals grind slowly
aDd require sbup. fresh abrasives. The recommendations of
grindin8 wheel manufacturers should be: followed closely for
rough grinding. Silicon carbide papers, usually run wet. wi!!
give a fiDCfinish. Papas should be: discarded f'rcquently to
prevent loaCina. Chemica! polishing preparations. while
relatively umried, may bave decided advantages in handling
these materials.
8.13.2 Solutions in Table 13 ate not diffieult to prepare
but involve the use of bydrofluoric acid. This acid <:an give
exucmcly serious, very painful burns. The HCI-HF solution
requires desaunung. The specimen sbould be rinsed between
etcbirag and c:tesmuttina (TabIe 13).
8.14 Zinc and Zinc A,1/o1s:
8.14.1 Zinc aad its alloys cold work rapidly and recry~'
talltte at low tempeJatun:s, th\lS allowing false structures to
Conn wily. Coarse-&rain= ~nc and zinc alloys are more
prone: to cold work thu IIOmeafthe fiDe grained die-casting
alloys. A good telt ror the presence or cold work, C$peciaHyin
coarse-grained samples, is the appearance of tWinning after
etcbing.
8.14.2 Samples should be cut with a $harp saw and.
sro\lnd on weU-Iubric:ated silicon carbide papers at slow
speeds.
IU4.3 M«fOelchflnu for Zinc and Zinc Ailops (Table J4:),
9. Keyword.
9.1 alloyS; eccbaD~ etching; macroecching; rnacroetchant;
macrostructure; metals
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1818 A8QI 51.. 1'ttI1tde/pIt/f, PA 1"/n.
10
TOTAL CC.11