ASTM B456 - Chemresearch

07/19/95
09:50
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DOCU11ENT
ENGINEERIN!3C.O.. INC. .; 5~5 892 1159
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,
St.ndard Specification 'or
Electrodeposlted Coatings of Copper Plus Nickel Plus
Chromiumand NIckelPlus Chromium1
Tb.. 8Iund.rd Is iuucd ul'd~r Ihi flud GealinallOIl a ~S61
,hi number1"""01118\.1)'
Ibllillllln Ibt CltII",allOlllnClhlllCS
th' ~r
,
orll'n.' Idoplioll or. in ,tit ca. or "..Ision. Ih. yeit 6( lu, revllinn.It.IIU",.' IIIpaNn'blllft MIl
II/PO"""P' ...il.n hI '"dlcl4,. III ,di'8ri.1 thllna. Ii,," ,he Iii' ""lllon or tCI,ptO,/II., '
Scope
J.
" J This specincatlon covers reQuircmenu
(ar Slveral
types and arudes of eJl!ctrodepo~itedcopper plus nickel plus
~hromium or nickel plus chromium coatin&t$
on'teel, nickel
ph~5chromium coatin.- on copper and copper aUo)l',and
C'opper
P'UI nickel plus f:hrontillm eoatinp on zinc8J10)'1
tor
applicationl where both appearanceand. protecllan of the
basil me&lllllinst carro.ion are imponant. Five artdes of
coltin,s .ra pravldedto correspond with the set'Yiceconditlonl underwhichneh is eJtpccted to provide sad.factory
performance:'namely. extended "cry severe,very severe,
Ryer,. modetate, ,nd mild. Dennidon~ and typical eumples
of ,hlle leJ'\lict conditions are pro\'ldltd in Appendi~
XI.
1.2 The rullowift&huards Clveatpenain. only tD the teat
mothods'ponions. Append;"..Xl, X3. and X4. or this
Dr
III' ,lIr arloft nlppro".,I, It.
B 487 T.11MethodI'or M.alufement of Metal and Oltide
CoatlnsThlekn*C8 by MicroscopIcsl£uminatlon ora
CrollSoction'
.
8 499 Teat Method (or Me.uremtat of Coadn. Thi,k.
. nO&8by the Maane\icMethod: NOftllllllftotic
Co.t.iltll
on Ma.netic Jnstt; M,tallI'
fbr Mcu~rnmlSln uf Thickn/:ss of
Metallic Coat'n.. by the CoulomlJlric:Method'
8 530 T.lt Me\hod for Mouurtmont of Coatins Tbi~lc.
a 504 Test Method
neuee by &heMapede Memed: I!lecirodeposi~
NIckel
Coatln.. Oft Mnlnetlc aDd Nonml8netic SubsltttesJ
B 537 Pra!rticcfor Ratin, of Elt.ctroplatedPanels Subjectedto AtmollphericExposurel
14554Guide for M~urcJ!tent of 1'h.lclcneuof MeWllc
COltln.. on Nonn1CtaJllc
Substrate,'
,
specification: This s'QltdtJ,d dots """purpOrt to addre:u d'i (Jj
itl,/iIJI CQn(~rnl. if alf)'. tl$S(Jcf4ted with iu wcf. II is the
rtJpOltilbi/ilJ' (Jf the JlICf ()f this IltJ.nda,d 10 ellfJblish fJpproprill" stlltt.\' I2nd hefl/th prattle,.s tJnd de"",,;n, the applica.
bility 0/ r~t~l/tllO"J'limiUll;()n.s prlfJr tQ uSt.
Non I-The tSO stand_rd&1436&ftd 145' are no! requir.tI\cntl
butun b; rcf8l',nctd,rot additionallnrormatiOIl.
B 568 Tut Method ror Mellurement of Coa\ina Thick.
nell by X-Ray Spcunrometry3
B 571 Tesl Methacil for AdhtlioJl ot MehllJi~Coati"..'
e 602TeAtMethodfot AttributeSlamplinlJ
af Metallic:and
Jnorpnic Coati11&1:1'
IS659 Ouldo ror MeBSurin~Thickneas of Metallic and
2. Refcrtnc:o(1Document~
B 691Quid! (or Selectionor SampllnaPIanofor h,.pee:.
110n of £I,elrodeposited Metallic: aDd Inorpnle
2.1 ASTM Stflndllras;
8 11,. rCSt Method ror Sal,t Spray (Faa) TOitina2
B 183Praeticcror P,reparation
bf Low-CarbonSteelrar
ElecuL~Ialina'
.
B 242 P"'t;tice for PrepatutitJn of Hip-Carbon $\011ror
ElectrapJatina'
B 252 Practiceror '~eparalion of Zinc:AllOYDie CUtin..
for EleetropJatina and Conver'ion Coatinp'
8 281 Prac1,jcefal' Preparauon of Copper and Copper base
Alla~'1for EJec:uoplatlnaand Conversion Coatings'
B 287 Method of Acetic:Aeid.Sal\ Spra)'.(Foa) Tesung. '.
B 320 Prattice, fbr Jlrepl\ration ot Iron CUtin.. ror
,
Coatinga)
,
,
a 762 Mtthod 01'VariablesSampLinlof M.ta11i~and
lnol'pnlc COAdlllpJ
a 764 Method tor SimultaneousThicknessand ElectrochemicalPotenual
Determination!)rhldividuallayers
'n Multilay.r NicklslD.po.h (STEP Te:ln)3
D 1193 Speclncation
tor a.a,.nt Wa1er'
S 380 Methodof Corro.lon Tc.th\1 of DecorativeEleetro.
pla\edeoltinas by tht: Cl)I'1'QdkoteProcedur.'
ISO I." Metallic lcoatinss-Electroplated coati"r of
copperplus nickel jpJuachromium 'iirtln or,lteel
I
Thil Iptclfia.lioll il unlltr lilt Jvri84/CIID"of ASTMComlllineeB.8 on
Mtullic ""tllnOlplllc CO&tin81Ind f8 1111"j,., IIIIOnll"lIIl~ or Ivbeoml'll'""
IOLO) 011DteortllYt COIIIIII',Nlcklf. OI'Ol'llilllll, I"d Nitk,loChromlloll'll COI'.
11\81.
tV""'1 Idilioll .~,tO..c.cI Ma,cll I.. 1994. Publlslled Mo, 1994. Oniinill~
Plllali"',I1...
.Sf. U. w, "'twiO",' ~4i,io" 1\45. - 9311.
. "'It'/ifli .,101; qf .tSrM S'lfnda,tI,.. YOI03.0~.
. '''''It/al
S...& rl( .1.'1'101 .~la"Jfltfl.r. Vol 02.0~.
" Dlaro/niny.,I-Sa
11/116AItIl'HlIIJI)(JJ;
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D39S' PractJ=(or C.ommerctaJ
Pj&cka&!ul\'
1:50 Pra~llces
for Apparatus, R~lelllll, and Safety'Pre-
B 368 Method for Copper-Acceterated Acetic!Acid-Salt
Spray(Fal) TcsUna',
---
loarpnlc CoatinpJ
cautionstor Chemica! Analyaiaelt Meulls'
2.2 ISO StaMQ,ds:
JSO1456M.callic cOtunas-ElIIIC1rod,potijted
coadnpof
nickel plus chromhlM and ot copper 1)lusnickel plus
chromium'
EleetroplBtinA'3
'
,
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DOC\J1'1EtiTENGINEERIN~ CO. I INC. ~ 505 892 1159
217/19/95 09:51
411}t
pa~3/012
8 456
TAIL! 1 SUMMa" of tile Aequlram."la lor Double- ",II T"pl.-La~~ HI.lctl C~.tII\O'
fIIlllIII811
cUo."".."
Steel
_71S
MICSGllilllllihaalJllU')
>0." 11'1""
TOil"'1
~O,O.."'In'
1D':'28
"
I.'~"
Trill
01 NIC'l8I
I_'ie
1I0IIgI,lon
...
BoIIOlll
T~ M.~
a.. ~~
..
XI
.111111' Coftt8ll'
-
AtltiiYiiOTOj; NICI(1t Tr\;;;'"...
. _.~
Doubl&-l.AJ8IP
0l1l8I'"
ftlplioL&ytt
81l1li
tnlf01",,11
-;~eo.
-'5o4Di
Jli101
-=:lDI
'0 0I
NOI.I'
1II0te40
,
A Copper WIdline:,lAMlr."1 .". tfttIt a_I.
. 'or NOI'I ., aM .. .. Seotlon e.
d -doubt.. ortripl..I.~.rfliek~1
~oalin&S
$uqalu thollsurflcunormallyvisible
3.1.1 J/",I/II:,.1I'
r -",1I11t (thilla, CCnYflllllollal)
ehtomilolm
(direc\Jy
or byrcnecdon)thatareessential
to theappearance
me -mictOCllcltld chromhlm
or .ervfceabllltyof the anicle when 811CmbledIn normal
mJl-mlotQporo". chrornlum
position:or that can belthe sourceor c:orrosionproductslhat
4.5Exampl,qf'CDmpl",
ClatlijlCtltiO"
NumbtrJ-A coat.
defice visible sul'f8CC$
ou the assembledarticle. When
nec:elllry,the II.nlOcant surracesshall be speeinedby the in. on Iteel comprilin. I' j.Lmminimum(ductileacid)
c:apperplus 2' 11mminimum (duplex)nickelplul0.25~m
purchuer and shall beIndicated
on the drawinp of the parts.
minimum (mlc~racked) chromiumhu the (:Iaulftcatlon
or by the pravilioft of lultabl)l markedsample..
number: Fe/tu15a NI2Sd Cr mc (- 4.3 and 6.1 for
.~pl.n.tion or Iymboll),
4. ct..,U1car1oft
,
4.1 FIvearaclol orcoatinas desiaoatod by service condition
ftumben and ..v.tI! types of coetin..dcO~edby classlfica. S. OrderinllnfoflDadolS,
S.I When ordenq uUcl.. to b. electroplated in conformtion numberaatecovuedby thi. speeincation.
4.2 Smlt, COlldillDnNumb":
aneewith this standard, the puroha.ser shall IIlIItethe rol..
lowing:
4.2.1 The 8trvlce condition numb.r indicatel the ..verity
'.1.1 The!ASTM de$iSnAtionnumber of thl~ Stt\ndatd.
of ejtpo$ure ror which the gradeor cOltlnaII Intended:
SC j extended .eycr~ $CJ'\tiec
,. '.2 Either theclUllOcaUonn&&m
ber or &fteIpcctnccoatIn, required (see 4.3) D' the lubltrlle maceri.a1 and thelOrvlt:e:
sC 4 very.,vert Hrvicc,
conditio" "\lmbet denotiq the Beyerityof the conditionsit
SC J "VIr. .'rYiCt,
is required to wlthltlnd (lee 4.2). If ttte !IOl'Vlce
~oncUtioft
SC 2 modentf. Ilf\llce.and
SC 1 mild service.
number is quoted alld not Ihe ellllint:ation nunlbet, the
4.2.2 Typical serviClcondition. for which the varioul manufacturer '5 free to supply Iny or the tYp6!1of cO8llnas
c:ot1'l!spcndin.to
servicecondition number! Ife appropriate are Jiven in d..lan.ted by thl claasificationnloJmbel'll
,
'
Appendix X I.
4.3 Comi", Claslijlc:atiQfI
Numb,r- The coAtil\8clwin.
cationnumbereomprtses:
4.3.1 The cliemlcal symbolrorthebui. meJaI(orforthe
principIImew It.n aUoy)~nowedby . .Iash
mark.
".3.2 The chemlcals)'mbol ror copper(Cu)(If capporIs
U&~d).
'
TABL.!I NI.tl "lullCllremlum
CoolIl\g' elt lta,l
ND'. 1-Au\IIt, 01. "" 1II'IIf1/ll1rlGlla1'Ultr't 18II)1\IImil'" wMUWIlI8
bII,IliII!a "y.'I""S
,
.am.
indicatln.theminhDumthicleness of the
4.1.1 A num~r
coppercoalinain micrometret(U'copper il used),
IIrvIot
4.3.4 A lower-cue letter designatlns tho t)'J)Cor co~per
deposit(ir Gopperil used) (se. 4." and 6.2.3),
4,3.5 The chernlcaJ uymbol ror nickel (Ni).
4,3.6 A number indic:atlnathe I'I\h'limumthickneaaorIhe
nickel coalin" in mic:rurnetre.,
4.1.7 A. lower~cue
lete.rdelianatln.thotypt of nickel
dCPQlit(see 4.4 find 6.2.4),
4.3.8 The cl\cmlcilsymbol rarchromium(Cr), and
4.3.9 A lotter (or leuors)deaianatin.
thetypoofchromham
,
~
and it. minimum thlckn... in micrometrCl(He 4.4
and 6.~.5).
,~.4 $)Jmbo/Jji),E.qJtlls/nt CltUl(j1tmIDfI-Th.faUowln,.
lowor-tase letten shall be used in c:OItln8c:laullic8tion
numbersto describetho ty. ot coatinil:
deposit
.
b
,.
dfllItIIlI6d
by IJ'II c~..slftca'iatl
nllmlj.,..
II'\w~~II'D 'UClutll cIwo
millm .,. uli'factorY for SC 4 IIId ~C 3.
Non 2-Whtn
pennllttCI till Ih. II\IfCNIIf, cop!* mill)' ~ Illed .. 811
undercoal/Of ttk:ktl bII' It noC !tuGtlih..1aDIefar ."y wt 01 "'" IIlcMj Iftj,knest
,pecllIed. If \l1li ~ 01 /!Oppel t. pCImIilttd, T.bIIt 3 till, 118ullOO10 oIal8in tho
-duc:tlle tc)~I~t,dej:lOSlted
r,orn.cid.t1fP8 baths
-sinllt-1aye1 I\lOkcldeposited in the fbllY.brialucondition
-dull or ltift\:-h"'ah. n~"cl rCQllirini pal:lhi... '0' &I-. tlil/
brisJuneu
"
ro.~1IOn..
CIfIGIIiM No.
Clt..IIIcI'1On NO." --
NIck81
1'1I1CICnIII.
1'111
8CI
so'.
sea
Crma
Fu/NI3$cf
Ct m~
,;
F"/N~011Of r
Fol"ll30c1
Ct me
PII/NI~OCI
er mp
.0
'o/Nidd
35
120
3D
FClINI~Ot
Cf,
30
21
Ffl/NIIIO
CrIl1O
"'/Nlllei Cr"'~
'
II
F./NMCJ
Ct,
8ca.
Ie
,.
" WIIaIIa &dItit ..d"
40
II"NI~O.
C,mo
'II/NI:.Op
Ct~
'e/NI2011
0, r
f:'JNII'~Cr1M
:10
30
:to
l'
Fefl'4l's.Cr 1'111
1.
0/,
-Ft/NIIOI
"""" IIIr"'.
""""'.
,
10
~
Dnldtl/ IIU, D8IIID8ulllt8lf
lOt a b ftlckll or lor IN IriOn' lI,er 01 d 1IIokII.
.. p 014 lI!ellal m.y De lutI"IMICII«
/\ICk. In SInice
CeIIcdllonHOt. I and
I, ~ m: ormpClVotnIwl'l
n'I8)'., lloIIIIcll\II8G
rill, Cftlanlum
In~
NO,I.
~tJOft
2
..
6S11-268 S0S
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N3A31S 'l'~ E1:21 S6. 61 lnr
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07/19/95
D~I8NT ENGINEERINGco., INC. ~ 505 892 11~~
09:51
4t
~
ClassIllCatlOn
No..
TABLE 5 NiCk.' Pltll t:hromlumCoaUng'"on r.ap~..' or COlllpt,
Alloy,
.
NIcktI'nIicknn.,
pm
.
SO 1\
sc.
SC3
"1/Cu'S.N"t3Od Cr "'°
Fe/Cu'S. NI3Od Cr mp
1ft/CutS. Ni25d Ct II'rC
30
30
25
Fe/OU'S, Ni25dcr "'P
FI/Cu,2a NJ2OdCf me
F8lCu12aNi:lOO
Or mil
25
20
20
.. WhIrl a d...11or lIalin 'InlShls
lor lhe bf"IGI'lIIIy8'( 01 IS nlck.l.
required.
""buffed
N~TI!-AItIICIu;h h
dUliftcltlan
~
are lIuarnctcry for UCft cf iI8
InCIiCIttel aervIcecandltICIn n\IIIW.. """'"'
are ;1I,.,.an~ IUperIor in ocrroCIIan ralltani:8
SMvieeCct1dItlcnNo.
SC4
UIinQ
n'iCJctRI=nI/n~. ~Ium
to 11'1010ua1118Ng!Aat ctIraINum.
Cl8WllcltIOnNo,A
CU/N13Od
Or,
II nickel may be IUI'ISliluled
1SC3
N1dc.,~nolll..
TABLE 4 CO"," PlUINick,1P/ul ChromiumtOltinlll' onZInc
.
.
Alloy
NOTi-Result$01. tosl program iMitate Ihal8 ill lome dOl/i'll wl'lttl'l.t lhe
coating systems de.etj~CI 1'1,th8 dll8lificedon IIlImllerS itIVOlvingrogutar C/Uoo
ServfoeConCli.tOIiNo,
SC S
.
~-
Clessl'lcatiOn No. ~
.
Nk1kel ThIcIInns.
2n/CIIS
set
SC3
N'135d Ci' nip
INCuS Ni351SCr r
Zn/Cu5 NI3OdCr mc
35
30
Zft/CIIS
NI3011 Ct mp
30
%n/CII5
1I/'25C1 CI' r
25
Zn/Cu5 Ni2DuCr me
Zn/Cu5 NI2OdCr mp
as
CU/Nl2Sd Cr 1111)
25
.
Cu/Nl25dCr,
25
.
SC2'
tn/CuS Ni2SpC'. mc
ZnJCu5 N125pCr I'll)
25
Ni3SP Cr r
tn/Cull NI2QbCr r
Zn/C5 Nasl'I Ct me
2n/Cu5 Ni1Sb Cr "'II
1. and I'N:or mp
dlromlun\
OulNi25p Cr r
Cu/N12OpCr me
CII/NI20p Cr Inp
20
CwJNi30bCr r
CuJNt2lib(irme
30
25
25
Cr mp
CIIJNI15D
C, ,
SOl'
~
Cu/Nl5b
Cr,
Whena dvllor otin
tllllllllt
,_8d,
--~~
.
28
20
1S
10
:
10
5
Ullbutlacsp nlC*f' may beIUrJ8UIllt~
t« tI niCkel or for tI1t Clrlfht 11)'" 01 d n1cIcll.
I P cr G nIt:okeimay be subllIMeCI fer b nlckll h SIW\riCI8CcnditIan NoI. 2 and
1 ~ me 01'mp cI1rcml\llllMat t)fraubstllUI8d fDr t ct\romILnTI InService~IOII
No.t.
in accordance with Method B 764 within the limits Bivenin
'5
6.7.
15
.
5.1.1J Adhesion Test-The
6.3)..
'0
" When . Gull Of sat!r'i FinIsh IS roqu.rOd. uJ\lIIIn~ p'niekelllllY
1:18lubSlit1.lttd
for b nICkel or for the brigMt llyer 01 d nlc:kel.
.
. p or ISnlck.1 t"tI., be IWbslitutlCl'OI b nldwlln Service ConditlOtt NOs. 2 and
No.t.
20
CuJNi10D Cr me
CU/NI10b Or mp.
20
.
%/l/Cu&Ni'DbCr,
so ,.
SC;!O
20
Cv{NI2Od Cr nip
CujNl25b
20
35
2S
nlCl/$
JIM
35
35
ZnlCuSNi35dCt I'IC
:SO
C\I{NI25d
Crme
Cu/N12Od C, me:
mum 8f1Ut!SIICtC/Y
lorSC. InllSC3.
1"'Id\O4/\Ql":
B 456
TABLE3 Copper Plul Nick., Plul Ch,omillm CoaUngl an Bt..,
StrvIceCondltiC1ll
NU.ll:Jb
adhe$lon test to be used (see
6. Product Requirements
6.1 VisualDdtcu:
6.1.J The sisnific.antsurfacesof the electroplated article
mly be substituted 'Of r tIIromlum In ServIcI Cl:lndluon
shaJJbe freeof cleatl)'visibleplatinsdefects,suchas blisten,
the specified
,. service conditionnumber,as JiveDin Tables2.
3, 4, or ::i. On request, the manufacturer shaJJ infonn the
purch8JC!:ofthe classification number of the coating applied.
5.1.3 The appearance required, roOrexample,bright,dull,
ot $Btin.Ahemalively, samples showina the required finish
or RInge of fini$h shaJl be supplied or approved by the
purchaser.
S.I.4 The IIlanHicantsurfaces, to be indicated on drawings
of the parts. or by !.he provision or suitably marked speci-
pits, rouihncsS. tracl($. aDduncoatedlUgs and shalldot be
sWncd or diSCDlored.On articles where a visible conlict
mark's unavoidable, its posi\ion shall be specHied by the
purchaser. The electroplated article shall be clean andfreeof
damale,
6.1.2 Defects in the surface of thc basis metal, such as
scratches, porosity, no~conductin8 Inclusion~, roll and die
marks, cold shuts, and cracks, ltIay advu~l)' affect the
appearance and the perfonnance Df coatings applied thereto
despite the observanc!: of the best electroplating practices.
AccordinsJy, the plater's responsibility for defects in tbe
coatins resultins frorn such conditions shall1:e walv~d.
mens (see 3.1).
S.1.S The poshions on significantsurfaces for rack or
contact marks, where such marks Ire unavoidable (see6.1.1).
5.1.6 The f:ktent to which defects shall be tolerated on
nonsignificant surfaces.
5.1.7 The ductility Ir other than the standard value (see
6.4).
5.1.8 The utent of tolerable surface deterioration after
corrosion testlna (sct!6.6.3).
.
appropriato Iimit8tJoas OD'\lcb basIJ mcral CX)oditioos.
6.2Processand CC)Aling
Requirernentt:
6.2.1 Proper prepantory prOC:edures and thorough
cieaniul of the basis metal surface are ~ssentia\ for satisfactory adhesioD and cOrTInlonperformanco of the coatins.
Accordingly, the applimtble praCticcsfor the preparatiDn of
various basis meWs for electroplatingshall be followed.
5.1.9 SampUnamethods and acceptanc:eIcvels(see Sec.
\ion
Nora 2-To minlmi2e,problemsor mis f~, the specifications
coven". the basismaterilJ0" the item to be electroplatedshouldconl.ain
7).
5.1.10 The minimum values orth~ electrochemical poten.
tial differences between individual nickellayeJ5 as measured
Various ASTM practiCC$ tor the preJlaracion of basis me",\
are available. See Section 2.
3
6£tt-268 £0£
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.." ..JI:J..J l:I:;Jc; 1.1 J::1
I
~"
41ftt B 4$8
the minimum thldcne$sof the nickelclecuodeposit at polnu
on the significant surface (see 3.1).
6.2.2 FOllowing the preparatory operations. the parts
(articles) to be electroplated arc introduced in s~ch plating
baths as required to producethe typesof depositS described
by the spec:if1ccoating c:fassiftC:lItian
numbers or one of the
coatins classification numbers listed in Tables 2, 3, 4, or 5
appropriate.for the specified set'lice condition number.
6.2.3 Type of Copper and Deposil Thlckness.6.2.3.1 Type o/Copper-The type ofeoppet is designated
by the ronowingsymbolsthat are placed after the thickness
value:
a for ductile copperdeposited from acid-type baths' containins additives that promote leveling by the copper deposit
'and that havean elonption not lessthan8 %.
6.2.5 Type 0/ ChromiumandDepositThickl'less:
6.2.5.1 Type 01 Chromium-The Iype or chromium de.
posit is designated by the fOllowina symbols phlcedaftet the
chemicalsymb.ol Cr: .
r for "regular" (that is, conventionaJ) chromium.
me for microcracked chromium, having More than 30
cant surface. The cracks shall be invisibleto the unaided
eye (see
~
6.2.3.2 Thicknejj 01 Copper Deporits- The number followina the c:helJ~ical symbol for copper (Cu) indicates in
micro metres the minimum thickness of the c:opper deposit at
significantsurfaces(see3.1).
6.2.4 Type of Nickel and Deposit Thickness.. .
6.2.4.1 Type of Nickel-The type of nickel is designated
by.tho fOliowinBsymbols,whi,b are placedafterthe thickness value (Note 5):
b for nickel deposited in the fully bright condition.
p ror dull or st~mi-bri&htnickel requiring polishlna to eave
full brightness. This niclccl shancontain less than 0.005
mass% sulfut (Notes3 and 4). and have an elongation of
not. less than 8 ~.
d for a double-layer or triple-layar nickel cOllins. The
bottom layer of this coating system shall a)ntain les.sthan
O.ooSmass% sulfur(Note4),andshanhavean elongation
of not less than 8 %. The top layer of this system shall
contain more than 0.04 mass% sulfur (Notcs 3 And 4),
and its thicknessshaUbe not IC$$than 10% of the total
nickel thlckMSS: the thickness of the bottom layer in
double-layer cQatinss shall not be [ess than 60 % of the
total nickel thickness, except (Ot steel. where it shall be at
leas17$ %. In triple-layer coatings. the bottom layer shall
be not less than SO% nor man: than 70 %. It there are
three layers, the intermediate layer shall contain not less
manufacturer.
nated by the coatitll elassUicahon number.
6.5.2 It is rea)gnlzcd cbat requirements 018)' exist (or
thicker coatings than are c.overedby this slJeCiflcalion.
6.S.3 The thicknessor a coating and iu various layers
shall be measured at paints on the slgnifi4::antsurfaces (Sel:
than 0.15 mass% sulfurand shall not exceed 10%of tbe
3.1 and Note S).
.
NOT!!
no simple method Is available for decenninlna ttle sulfur COntent or a
nickel depQsit on a coated article. chl:mlc:a1determinations are possibll
usina speciaJly pnpared test specimens (HI! Appendix X3).
NOtE 4-t~ will usually be IIOssible10 idl!lItify the t)/lle of nickel by
microscopical CJlarnlnation or lhe polished and Itched section or an
Ilrticle i>replred In ILCcOrdalletwith Test Memed8481. The thickneu or
the individual nickel la~el$ in double-layer. and tIi!)lc.la)'Clrcoatinl\.!. as
well II Ihe ele~uoehemlcaJ relaliol\$hips between thl! Individu" laycr.!.
eliI'!al$o be mell$lIred by Ihe STEP test.' in accordance wilh Method
8764.
.
..
6.2.4.2 Thick111U Df Nickel Otpotil- The number rollowing the chemical symbol Ni indicates. in micrometn:s,
6.5.3.2Thc micro$CopiaJ method describc:d in Test
Me&hodB 487 may be used to measure
thethictmess
of each
nfckellayerandof thecopper layer.
6.S.3.3 The X-ray method described in Test Method
B 568 may be used whenthe total thickness -clfa coppetl
'HmuIDk.
E. P.. "Simulttnecl'" T1titkncsa and EleCltOI:l\emicDIPOlenli:ll
Oclcnnlnallon of Il\di..idu:lll.Q~etl in Mullil:aver N'relt.1 ~pOsils,' PltJI'"R Qlld
S"r/IIC/!
I'1nl.r/,;",.
Vol 67. No. 49. February
..
L'd
.
5-When slanificantsurfacesare 1Jwolvtdon which (he
spcciOcdthickness ot deposit cannot readilYbe controlled.such as
Ulreads, koles. deep teCCSSCt,
bws or an&les.!I\!Idsimilar ara&, 1I1e
purchaseundthe manufactutlt should r8C0anluU,cnc<.~!SSity
rorlither
s\tr(accs Of for spcciaJ r:ilckin8.
thicker dcposll$011thc more ac:c:essIble
Specialricks mlY Involvc~hcU5Cor conrolTltlng.aUliiliary.or bipolar
eleeU'Odes
or ft<lDl:ollduct!nlst\ie1d8.
.
6.S.3.1 The coulometricmethoddesclibedin Methoc:t
B 504 may be used to lt1e.uurethicknessof the chromium.
the total thickness or the nickel, and the thkkness of the
copper. The STEP test. Method B 7641 whicl\ is similar to
the coulometric: method, may be used 10 c:losely estimate the
thicknesses of Indillidual layers of nickel in Ii multilayer
c:olning.
NOTE3- rhe sullUrconteIllSan specifiedin ordor ~oindicatewhich
typeor nickllelmvoplatins sol"uon must ha used. AlthouSh at pracnt.
-
.
6.S Coaling Thlckne.rs: .
6.S.1 The minimum coltin, thickne$SshaJJbe IS desig-
tOtaJ nickel thickness. These' requirements for multilayer
nickelcoatin...o;
aresummaritedin TableI. .
6.9).
mp for microporou$chromium containinga minimum of
.10000 pores/lO mm b1' 10mm square (LO000 em1). The
pores shall
Invisible to the unaided eye (lite 6.9).
6.2.5.2 Thicknell of Chrom{umDepos/r- Theminimum
thicknessof the chrami\lm deposit shall be 0,25 11mon
si&nificantsurfaces (see 3.1),exceptthat for servicecondition
SC I (see4.2.1) the minimum thicknessmay be reducedto
O. f 3 ~un. The thickness of chromiunt is designated by the
same symbol as the type,irlstead of by numerals as in the case
of copper and nickel.
6.3 Adhl$(on- The coatins shall be 5ufficltmtlyadherent
to the basis metal, and the separate layers of multilayer
coatingssbanbe sufficiently. adherentto each otber.to pass
the appropriate tC!$t$
detajled in Test Method$B 571. The
by the
particular test or tests to be used shall be spc~cif1ed
purchaser.
6.4 DUClililjl- The ductility shalt be such that theelongation will not be less than stated in 6.2.3.1ror copper and
6.2.4.1for nickel when tested by the method gjven In
Appendix.X2. Greaterelongationmay be requestedbut shall
be subject to asrcement between the purchaserand the
No symbol is placedafterthe thicknessvalueif a minImum elansatlon Is not requiredor if a deposit from a
non-levelingbath is permiued. .
. pointson
in any direction over the whoLe of the silnifi.
cracks/mm
1980.
4
6S11-268 S0S
N3A31S 'l'~ 91:21 S6, 61 lnr
------
,
£17/19/95
1i1=':~,j
I'!U.
UUCUM~NI ~NblN~~~lNb LU.. IN~. ~ ~~~ ~~~ !!~~
J.OQ
r\:J"-'Qr
\:JJ."-
,iii B4SS
Thc STEP pountial differencebclwec;n
nickel/chromiumcomposite coating is to be measured,
withoUI an)' indication of tbe thickness of eachindividual
layer;
"
6.5.3.4 Other methods may be used if it can be demon.
stratcd that tt\e uncC:J1.ainty
of the measurement is less than
10%, or lessthan that of any applicablemethod mentioned
in 6.S.3.0Iher methodsarc outJint:din Guide B 659. .
6.6 Corrosion TeSt;ng:
6.6.1 Coaled arlides shall be subjected to the COlTosion
. teSIfor a period Dftime that is appropriate for the panicular
service condition n.:amber (or for the service condition
number corrcsponding to a specified class.ification number)
6.8Sul/urCo",ent:
6.8.1 The sulfur content of the nickl:I dc~po$itshaltmeet
the maximum' or minimum vaJues as JUttedin 6,2.4.1 Ind
as shown in Table 6. The test is ()esc:ribed in detail in the
referenctd ASTM desianation.
NOTE 6- There is nc direct relation betweenthe reslIlu or an
Table I.
.ct~lerated «:ol'1oslonleSI "nd the rlSiSl3ncr to toITosion in other mcdia.
be~allse seve:ral f.clorl. sueh as the fonnadon of protecUvI films.
'nnllenc:t Iht pro&fCSSof cOITOiionand vary areatl)' with the eonditions
enrounlel'td. The resuh5 obtained in the: tlsl should. thererore. nol be
rc:,:ndC!d as a direel (luidll to Ihe c:onosion rtsisl:t.n~ of Ihe: ICSled
malenals In all envitOnmenlSwherethese m~nerialsmay be used. AI50.
perfotmance: or ditTerenl malerial, in thl tesl cannOI always be taken as
a dire"l &uide10the relative tesislanceof Ihesemalen;lIsin service.
6.6.2 After the anide has been subjected 10 the treatment
described in \he relevant corrosion test method. it' shall be
examined (or corrosion of the basis metal or blistering of the
coatin&. Any basis metal eorrosion or blistering of the
coatins shall be cause for rejection. It is to be understood that
occasional widely scattered, small corrosion defects may be
.
"1.Samplina
the function of the electroplatedpart. A method of ratina
a 537.
i.1 The
6.6.3 Surfacedeteriorationof the coatini itselfis expected
to occur during the testins of some types of coatinls. The
invisible
tD
Requirements
samp1ini ptan used for lhe .Inspectionof a
quantity of coated articles Shan be as agreed upon by the
purchaser and supplier.
utent to which such surface deterioration will be toJerated
shallbe speclnedby the purchaser.
NOT'; 8-Usually, who" a eollll::uon or CO'ated
anlcl", Iho inspection
lot (8.2). is eltlmlnedfor compliance with the l'8Qul~menlS,laerG on
the cDatina. a relativelyamaJl
Dumber of 'he .mcles. the sample!.is
scI~tcd II random and is hl3pected. The inspection 101as \hen classined
IS complying or not comptyiaa with dill requirem.nts baaed on the
results of ~heinspection af 11\,ample. The sl~eor ~hlf iIiIImpJe andIhe
,criteria orcompliance .8111determined by the appllc:allon of stalistics.
TIle procaduR! is knownas amplin. Inspecr.ion.Thnte standards. Yesl
6.7 ST,~P j~$r Requirements:
6.1.1 The electrochemical potential differences between
individual nickel layers shall be measured for muJtilayer
coalings c:ormpond1ha to SC5. SC4, and SC3 in accordance
with Method B i64 (STEP Tesl).
MethodB602,Guide8691. Incl MethodB '/62 <:011141" somplinaplans
NOT£ 7-Un;vtr$aUy accepltd STEP values havt 1101beln eslabliihtd but someagteement in Ihe value of ranaeshas been obLained. The
STEP 'Valuts del,end upon which two nickell.ycn are bein. measured.
TABLE & Corro.lon
The cracks and pores shitlllx:
,
mean that such defects are not, when viewed
is ,.iven in Pmctice
surface,
the unaided eye.
6.9.2 Methods for measurin8 the di~Ohtil1uit.iesIIrcth,cn
in Appendix X4. See X4.4 in Appendix. X4 for a meansof
detenniningQct;vecorrosion sites by COITOsiol'l
t!lstins.
critically,slenificantiydefaclna or otherwise deJeterious to
cortosion
6.8.2 Methods for sulfur dctemlinatlons are given in
Appendix X3.
6.9 Dens;ty and Measurementof tile Di.5continu;liesin
Chromium:
6.9.1 'The density or cracks Dr pore$ in microcracked or
microporous chronlium deposits slutll meet minimum
vaJues. Microcracked
chromium shall have more than 30
cracks/mm(300 crac~ks/cm)in Anydirection over ,he whole
of the significant surface. Mi~rOPi3rouschromium shall
contain a minimum or JO000 pores/IOb:l 10 mm square
(to 000 pores/em;') in any direction over me whole of the
significant
observed after the teatina period. In general, "acceptable
res.istance" Jhall
the: seml-briE'.ht nieltellll)"!r
and Ihe bri8ht nickel la)'Cr lias 8 ftlnlt 1)( 100 to 200 mY. For all
combinations or nlekellaym. mo scml-brisJtl nicklilayer Is mOR noble
(C8thodic) than the briaht nlcket layer.
The StEP pOtential difference between the hIJh-a.cti\'ity ui«:kellayer
and the briJht nickeillyer In Uiplc-Iayer cn.lJnas 111,\a potentlAl.1Inge
or I S to " mY. The hiah-ac:tMt)' nickel 11)'lIrIs nlora active (anodic)
than the bliSht nickell.)'If.
The STEP potlntial differeDu bllween the brisht Dickell.)'Ir and ..
nickeillyer
belwccn me bright nickcll.ytr
and the cbromlum layer has
. polen1ialranae oro to 30 mY. The bri8ht nleblla)'er Is morc ao1ivc
(anodic) than th~ mckel laYITprior to ebromium.
that are desi8ned for the IIRlplins Inspecti(1I) of coatinf,$.
Tat Melhod B 602contains(our umplinl plans, three for IIU wbh
T..,. Appropri.te
torEach Stryl~.
COndition NUMbtr
NOT£ 1-The I~ed
'"",1"" ISllspray IC'SI,TISI Melhod8117 "*' bIIenQlntlf'8I1y
ClIlCired1tlCllIS
an 1CCIII..111Id CORVSIon1151lor cJeconItlve "1cklf.d\romlURI
COllings IArge~ t1eC"4I1S.
01t.Ck 01"plodIICibifily 01 ,esulIS,"lIla r8cQgn1zed. ftOwlver. Ihllilhe tl""
tllU UHISIn 8OR'IIMglftllllt.
01Il1o l!Ic1rcpl8brlQ ,""u,.ry 10 CIIedc
11\. tju.fity 01 COII/J\gs 1t\lelldeG '011118 wn"" rellllvely II\ItI $Inrlct COIICIition1. ~ly.111a
SUOIIlltId ~I any u.. of IlIIt ttltllMlllf18
r8Q\riItmtmlS tu balMl De the
euajeel 1)1'egrll8lllQl\1 bet"'Mn
1118PJICh""
1Mb
manullClwrtr
and. furthIII'. thai il8 we be canfinecl to the CDI'lrlQt IndIcaIld .. tppI~111'
to' Serlica CQndIIIIII'II
Nos.2aI1d1.
'
Non
2-Tne
'AC81ic;'s8lt Melhod 8287 has been 1IIscon1inl/ld.
6eMco Onllian
8asIsMtI.I.
NO.
'
SC5
SC 4
~3
SlteII, me. ,/loy.
Cr copper .rId
,
g)Dpet IUoy
sca
SC1
,. MlndiUI. A...Slal'ldardSill.Spray Te'I-ls
It. Valid Ac:oeptance fe',?
Caro8Ion-;:;11nd
CASt MIIhOd
ISH
44
ft
d
CIc:mIc1kOII
IJutaIlorl h
Me\hocl
B 380
TWII18-1tCytIe&
~
...
PropertJ... T'81111114PerfORnlrlC801 E~odeposl'lId
---,
Acetl(:ollllt MllhOd B 287
'144
H
1!4
8
M18lldUc
CoatlnUI. ASTM STP liT.
ASTM t8~G. p. 107.
S
6S11-268
8'd
--------
- - - -
---
S0S
N3A31S .l'~ 81:21 S6. 61 lnr
-----------
0'7/19/95
09:54
DOCUMENTENGINEERING CO.,
4.
~
::'\:j:::! C!:!;:: 11:::!~
I'~IJ. It:Jb
t"""'" (" "'J.":
B 456
time under essentially Identical conditions, ~nd that afft
le5\s thaI An: n6n~e$tNttivt and one when thc)' II~ dcstNctivc. The
buyer and seller may asree on the plan Ot plans to b.! used. Ir they do
noi. Test Method.8 602 Identities the plan to used.
Guide B 691 provides I carp number of plans and also a!ves ,uidanee
on the sell:l:lion of ~ plan. When Ouidc 8 697 is sptl;incd. the b\lycr IInd
teller need to a&reoon the "llIn 10 be used.
Method B 762 ell" be used only for coatltlC requirements Ihat ha1lCa
nlimeriC41 IImi" such U C:OItinll thicknas. The lest must yield 11
n\lmericaJ value nnd "ruin
slatisticaJ req\liremencs must be met.
Method B 762 contains Sl:vctal plans and also &ivC$instl'UctioRS for
ealeulatin. plan. to meet soeeiQJ needs. Tile buyer Illd UIo sellet may
IlJtee on the pilln or plans to be USId.If lhay do not. 8 76.1 Identities Ihe
plan to be used.
NOTE
INL;.
submittedfor acceptanceor rejectionas a group.
7.3 If separatetest specimens
arc used 10 r.cpresent the
coated anlcles in a test. tbl~specimens shall be of the nature,
!!I~e,and number and be prcx:essedas tecluiredilt AppendixesX2, X3, and X4. Unlessa need canbedemonstrated.
separately prepared specimens shall not be used In place of
production items for nondestructive tests and visuIl1exami.
nation. for destructivetestS includins determination of ad.
hesion, ductility, sulfur contents. the number of discontlnu\.
ties, and corrosiontestinl. separately
pn,pan:d specimens
maybe used.
9-Whcn both destructivaand .nondatructivi testa exist ror
the mc~uremClnt of. c:haraCkris\ic. the purchaser needl to state which
is to be used SOIhe proper samplinl plan i5 scllcled. A test may. de"roy
the coatill8 but in a nonc:ritica1arca; Ot, althou8h it may desiroy the
coatlnL a lested part may be reclaiMed by sttippins and rec:oalJn.. The
purcllnscr needs to state whether the IC$tis to be considered destNctivc
or nondestftlctlve.
I. Packagina
8.1 Pans plated for the:U.S. Oovemment and military.
inc:ludinssubcontracts, shall bepackaged
in accordance
with
Practice
7.2 An insPectionlot shall be defined as Ii collection of
coated articlesthat are ot the same kind, that have beCD
producedto the same specifications,that have been coated
by It sin&.lesupplier at one time or approximately the same
D 39S 1.
9. K.)'Words
9.t corrosion:decorative;eiettrodeposited c:hromiumi
elec:uodeposited copper, electrode posited niCkel
APPENDIXES
(NonmandBtory InformatloQ)
XI, DEFINITIONS AND EXAMPLES OF SERVICE CONDITIONS FOR WHICH THE VAR10US SERVICE
CONDITION NUMBERS ARE APPROPRIATE
XI.) Se~/ct Condition No. SC j (Severe)-Exposure
. XI.I Service Condition No. SC j (Extended VII')' Stvere)-Service conditions that include likely damaacfrom
dentin.. scratchJnl, and abrasive wear in addition to expo.-
sure to corrosive environments
where long-time protection
that is likely to include oc:c:<a.sionai Ot tre~uel'lt w~tting by rain
or dew or possibly strona cleaners and saline 5Olutlons~for
exampic, conditions encounteredby porch and lawn furniture: bicycle and perambulator pan$i hClspitalfurniture and
of
the substrate is required; for example, conditions encoun.
teredby Some"tenor componentsof automobiles.
fixtures.
.
.
X 1.4ServiceConditic)1I
No.SC2 (Modertlle)-ExpoSUrCI
indoorsin placeswherecondensation
of nmisturemay
occur;forexampte,in kitchensandbathroom~.
X 1.5ServiceConditionNt).SC I (Mild)-Ey,posure indoorsin nannall)' warm, dry atmospheres
v.-ithcoating
subjectto minimum wearor abrasion.
XI.2 COlldlttonNo. SC 4 (Very Severe)-Servlce condi.
tions that Il\clude1ikelydamagefrolll dentin.. scratchina,
and abrasivtIwc:prin addition to exposure10 corrosive
environmentSi for example, conditions encountered by ute.
. riorcomponentsQfautomobilesand byboatnningsin salt
water service.
Xl- DUcrlLlTY TEST
NOT!!XZ.I- Th.ls lest is used 10 ensul'O cQmplianec or the typil or
topper and nickel d.er>ositwitb !hI appropriale dlfinilian &i\'Cftin 6.4.
with a nat shear. Round or chamfer the longer edgtS of the
strip, at least on the electroplated side, by C41'I~fuI
filing 01'
Jrindlns.
X2.2 Procedure-Bend the test strip whh the electroplated side In tenGloG
(C1I1the outside), by steadilyapplyins
pressure, through l80. over a mandrel of I LS mm diameter
until the Cwoends or the test strip are pa(;~lIel.Ensure that
contact between the test scrip and the n,andrel illm~~ntained
durina bending.
X2.3 As.sessmenl-The
electroplatlns is deemed 10
cOlUplywith the minimum requirement of an elongation of
8 % if after~"tina ther~are no cracksP8.&Sina
completely
across the con\"exsurface. SmaJlcracksat theedgesdo not
slanity failllA:.
X2.' Preparation
ofTen Piece:
X2.i.l Prcpar~an electroplatedtest strip, ISOmm (onl.
10rnm wide, and 1 rom thick by the followingmethod:
X2. 1.1.l Polish a sheet or the appropriate basis metal,
similar to that of the a!ticles bein, electroplated, eJtcept that
If the basismota!is zinc alloy.thesheetmay be:of softb~,
(Use a sheet sufficlentl)fIBraeto aJlow the test strip to be cut
~
from itScent$rafter trimming ofTa border25 mm wideall
around.r Electroplate the polished cide of the sheet with
copper or nickel to a thickness or 25 ~m under the same con.
ditions andin thesamebath 81 the corresponding articles.
X2.J.J.2 Cut the te3t.$trip from the: cl~c:troplatcd shect
6
6'd
~-
--
6S~~-268S0S N3A315 'l'~ 02:2~ S6. 6~ lnr
--
07/19/95
09:55
DUCUM~NI ~N~lN~~~INb CU.. INC. ~ ~~~ ~~~ 11~~
.
I:;JJ.~
NICKEL (NO1"E X3.I)
The roUowir'l&twomethodsforthe determinationof sulfur
in electroplated nickel arc given as guidelines for use to test
compliance of the type of nickel deposit with the appropriate
dclinltioneJven In 6.3.:2,They representmethods that have
been used with success commercially; they 8rc not ASTM
standards, nor is It the intent in publishing these methods to
preclude the use of other methods or variotions in these
Methods,
..
900 mL Dfwater and dilute to t t.
X3.I.S.1 Polauium Iodate,StandardSolution B (1 mL0.02 mil S)- Tnansfer 200 ntL of potassium iodatlt Solution
X3.1 TOlal Sulfur in Electroplated Nickel by CombusUon-
mustbe deltnnlnerJ by
.
A (I mL
0.1 ms S) tg a 1.L volumetricflask,dilute to
NOTEXJ.2- Tht sulfur equivalentIabll3el:lon .he completec:cmvcrsion of sulfur to sullUr dio~dde. The I'ecOY'I'yof uul(ur as the dioxide
may be lessthan 100$, ')\.Itit II consistent 1~hcn the \emperlt\lre and
the rate of OA)1en now Ire malnwneCI eonslant, An ompiricalfaeaor
IodateTilr.1io"
Bivenapparatusand for day.,;to-day
\'ariationin the
lilt
volume. and mix.
ah analysisor 8 standard $ample.
.
X3.1.S.8 Sla'ch-/odide SolUIIDn-1'ransfer t 8 of soluble
or arrowroot starch to a small beaker.add 2 mL of water,
and stir until a smQothpaste is obtained.Pour the mixture
infO SO mL of baiting water. Cool, add l.!i I of po~sium
iodide (KJ)\ stir until dJssol\'ed, and dilute to 100 mL.
X3.1.1 Stope-This methodcoversthe detennlnation of
sulfur in concentrations from 0.005 to O.S mass %.
X3.1.2 Swmmary of Melhod-A major pan or the sulfur
in the sanlple is converted to sulfur dioxide (SO2) by
combustion in a slrtam or oxygen using an induction
futnlce. During the combustion, ,be SO1 is absorbed in an
acidified 5Utrcb-jodidesolution and titrated with potassium
iodate Solulion, The latt~r is standardized against stcels of
known sulfur con~ent to compensatefor characteristi~ of a
.
rl:Jl:Jc'
B 458
X3. DETERMJNA TlON OF SULFUR IN ELECfRODEPOSITED
.
I'II.J, J.ClO
X3.t.S.9 Tin (lowaugur)AcceJel'lItor,
sranular.
X3.1.6Slalfdards-5tandards fol' cal.ibrationare National
Institute of Standardsaod Technology$\"1$of the proper
sulfurcontent.
X3.1.7 SamplePrepa'ation:
X3.1.7.1 Pn:paR!"test panel or cold-rolledsteel ISOmm
Ions by 100 mm wide by t mm thick or any other
convenient site. C1e;t.n.IIQid dip, and ,~lec1.roplate
with
per.
centaaeof sulfur recoycred as 802, Compcnsadon is made
(ot the blank because of accelerators and crucibles.
approxlmatClly7.S ~m of an adherent nickel deposit and
thoroushlYrinse. ButTednickel or buffed ttainless steel may
alsobe used asa1tel118ttves
to steelelectroplatedwithnickel.
X3.1.7.2 Passi'iate the test panel unCldicaJlyat 3 V for 5 to
10 s in a hot alkaline cleaner (~perature 70 to 80.C)
X3.1.3 lnrerfereficcs- The elturlen\Sordinarily present in
containing
30slL of aodJum
hydroxide(NaOH) and 30 &lL
electroplated nickel do not interfere.
of trisodiumphosphate (Na3PO.,or 60 8IL or aD)'o&hcr
X3.I,.4 Apparatus-Induction heatina apparatus for de.
suitable anodicaUcWine
cleucr.
termination of sulfur by directcombustionas describedin
X3.1.1.3Coattbepassivated
Ie$!panel '\lith 25 to 37J1m
. Practices E 50 (Apparatus No. 13).
or
nickel
deposited
from
the
same
soluda" using tbe same
X3.I.S Reagenl$:
. .
X3.I.S.1 Purity of Rtagenu-Reagent grade chemicals parameters as for the coated artitlCtIrepresentedby tht test
specimen.
sha1l be'i.lsed in all tests. Unle$S otherwise indicated, it is
X3.1.7.4 Remove the edges of the et~troplated panel
intended that all magcnts shalt contonn to the Specifications
with a hand or power shear or any othl."famycnicnt method
. of the Comlniuee on AnaJytical Rea,ents of the American
Chemical Society. where such Specifications are available.1o that permits readyseparationof the tes' fail
x3.\.7.S Separationfrom the palDel, wn1htbe rilckel foil
Other grades may be used. provided it is first determined that
electroplatewithwaterto removesaltsBndbiOidry. Cut into
the reagent is of sufficiently hiah purity to pennit its use
pieces 2 to 3 mm J'tr side with a sdssol'lc.Transfer to a
. without lesseningthe accuracyof the determination.
X3.) .S.2 Purit)' of Water-Unless otherwise indicated, IOO.mL beaker, cover with water, and heat 'o boiling.Pour
off tbe water and wash with methanol. Air dry the nlclc(!1on
reference to water shaU be understood to mean reagent water
filter paper.
.
. conforming to Specification D 1193.
X3.J.8 Weight /0" Standards and $amJ'ies,-Select aDd
X3.I.S.3 Hydrochloric Acid (J""97)-Mi'l
3 volumes of
welsh to the nearest 0, I mg an amonn, of !Mlmpleas follows:
concentrated hydrochloric acid (HC!) (sp 8t J.l9) with 97
EXI*1H SulfurConlcn"
volumes of water.
Non X3.1-lnstrumentsore a\'ailablefor .tneasurin&
the sull'ur
dlo~idefrom combustionby Inrrareddeteetiot\methodsand uun.
built.incomputen to Intesraleand displaythe.lull'ur cantontas a
pen:entage.
MUS~
0.005to 0.10
0.10100.$0
X3.I.S.4 Iron (LOw-Sf.if"r) .Accel~'QlOr-Chips;
X3.U.S Iron (Low-Sulfur) Accelerator-Powder.
X3.I.S.6 Potassium loda(e. Standard Solulion A ( J mtO.t
WCi~1ofSanlplt..
I,CI:I:0,02
0,:1!t.O.C:U
X3.1.9 CdlibratiOfl-Sclcct a minimum (If two standards
with sulfur contents ntar the high,.and low-limitsof the
ranse tor a given sample weiJht and also onc: near the mean,
The meanstandard may be simulated, if necessary,by taking
onc-half the sample wci&ht of each or the other two. Follow
mBS)-Dis50lve 0.22.25&or pl)tWium iodate(KJo.,) In
10-Reoaenl Chemlells, AmC':rltln ClleMteal Sociel)' Spctll1callOlls," AM.
Chemical Soc:.. Weshil\&ton. DC. For '1IlIlISlions an the Irtlina or tOIsenl. nOt
listed by Ih, "Mericln f.bemlcal Socld)'. see -Rea",nl Clltmical. and Slandards,.
~ Joseph AOlin. O. Villi Nostrlllld.Co.. Ine.. Naw Vorlc. NY. Rnd the .Unlled
StalA PII\lr"'.co~ia. - .
thestepsofthepr~ure.
"3.1.10I'r(Jcedure:
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X3.I.IO.1 To the crucible add I g of iron chips, 0.8 g of
Iron powder, and 0.9 8 of tin. Transfet' the proper weight of
sampleand covt:r.
.
X3.1.10.2 Turn on the power of the induction furnace
and anow the unit to heat to' operating temperature. With
oxnen flowln, through the absorption vessc:l, fill it to a
predetermined point with HCl (3+91) (X3.1.$.3) (Note
X3.3). Add 2 mL or starch solution to the vessel. With the
oxysen flow adjusted to 1.0 to 1.5 Llrnin (Note X3.4). add
KIO) solution specIfieduntil the intensity of the blue color is
that which is consideredas the end point. Refillthe buret.
R€C!lvIIoiG
FLASI(
811the titration ve&:l to the samepOint.
NOTt X3.3-AlwIYs
Non. )(3.4- Tbe OX1B~nRow nil may be adjusted10 meet the
requitcmel'llSof individutl openllors or equipment: however. tho now
ra&lmuSibe the SaMefor me test samples and ,hi s1andard$l\mples.
0
X3. I, 10.3 After the unit hu been at opcratins tempera~
ture for at least 4' s. place the covered crucible containing
the sample and acceleraton on the pcdeml. Witb the o)t)'scn
now adjusted,raisetho crucible. close the f'urnaco,ttnd tum
on the power. Bum the sample fot 8 to 10 min. Titrate
continuousty with the KIO) solution at such a nne as to
maintain 85 nearly as pO5.siblethe oriainallntenslty of the
blue color. The end point is reached when the ori&lnalblue
color is stable for I min. Recordthe final bun:t readins and
.
FIG. X3.1 App.r.",. ror Ihe DeterminllUonQf$\llf," In
EI.~pl.tld Nick"Foilb~thl EVDluUon
M,UlocI .X3.2
drain the titratIoD vessel throu&h the exhaust stopcock.
X3.2.2 Summaryof MethodII-Sulfide sulfur is evolved
as hydrasen sulfide (H25) on dissolvina. the sample of
hydrochloric acid' (HCt) containini a smaU amount of
X3.I.IO.4 Blank-Detennine the blank by placing the
.
same amount of accelerator.; used In the test sample in II
preignited crucible. Covet and proceed as in X3.1.10.3.
X3.l.11 Calculation-Calculate the sulfur faCtot of the
. potaSSiumiodate asfollows:
platinum as an accelerator for dissofution.The sulfur is
precipitatedas un!: sulfide(ZnS) in the receiving vc~s.seland
then titrated with standard powslum iodate solution. Values
arc based on potassium iodate (KJOJ) as the primary
Sul(ur
.-
(actor.
standard.
aluni' ...alume- (C _AD~
: 100
where:
If'
B
C
grams of Standard sample used.
percent$uIrurin thestandardsample
X3.2.3Apparatus:
X3.2.3.1The apparatus is shown in Fig. X3. J. 11may be
assembled
usinsa SO-mLErlcnmeyet f1a:skwith a No. 19/38
.
- mtUilitres of KIO)solutionrequiredfortitration of the
outer joint. A washbottle fitting with a No. t 9/38 inner joint
~Q be :cut to fit the SO-1uLnask. The exit tubctcan be bent
and c:onn~tcd to the 6.mnl aas tube with tubing.
XJ.1.3.2 A nitrogen cylinder with valyes and prcS$ure
standaflt sample {Note X3.S), and
D - miJIIlitresofKIO, solution required for titration ofthe
blank (Notl X3.S).
regulator.
X3.2.3.3
a"parel11 percentase
or sulfur (Ot -direct-readina-
NOTE XU-Or
burets.
.
X3.1.11.1
Mmple as
X3.2.4 Reagtltts:
X3.2.4.1 PurilY of Reagents-Reagent aradt. chemicals
shaDbe usediD au testS.Unless Qtherwisuindicated, il is
intendedthat aUreagentsshaDconformto the specifications
of the Committee on Analytical Reagents of tbe American
Chemical Society, wheresuch $pecHicationsare available.1
Otber &tadesmay be used, J~rovided It 1$first ascertained Ihat
the reagentis of sufficientlyhi8h purity to permit its use
without lessenlna the accuracy of the detennina.tiQh.
CaI<:ulate the percentage of sulfur in the test
follows:
SulfUr. mass"
where:
.
(E -D)F
G
x 100
.
E .. KlO) solulionrequiredfor titration of the test sample
(NoteX3.S),mL,
.
D "" KIO, solution requiredfor titration of the blank. mL,
F II: averaae sulfur factor of the KIO, for the standards
used (see X3.J.lI), gfunit volume. and
G - sample used, 8.
X3.2.4.2Purity of Wate,-Unless othCl'WiR.
indicated.
reference
to watershallbeunderstood
to meanreagent
water
conformina to Specification D 1193.
X3.2.4,3 AmmoniacalZinc Sulfate $orllfio1l-.DiS:lolveSO
g ohine sulfate (ZnSO... 7H:sO) In 2S0 mL orwator. tdd 2'0
mL ofammo&\ium hydroxide (NH"OH, sp it 0.90) and mix.
X3.Z DetermlnatioQof Sulfur in Electroplated NIckel by the
---
Evolution
.
Buret,:to-mL.
Mechocl
X3.2.1 SttJpt- This methodcoversthedeterminationof
sulfide sulfur in electroplated nickel in the range from 0.005
"Lllk., C.I...
. to 0.2 mass CRt.
A"alYlletlIChtrniJIIJ'. VoIZ9. 19'1.11. ';!27.
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Transfer 10 a Rask and anow to stand about 24 h and filter
hexachloroplatinlc
inlo a polyethylene bottle.
Xl2.4.4 Hexachlotoplatint'cAcid SolutiO1l(JO g/L)Dissotvc 0.5 8 of hclt&chloroplatlnicacid (H2P1C16.6H2O) in
about 40 mL of water. add S mL of hydrochloric:acid (HCI
Sp gr 1.19). ftnd dilute to 50 mL.
X3.2.4.' Hydrochloric Atid.PltJlillum Chloride Solu.
lion-Prepare SOOmL of diluted hydrochloric acid(HCIsp
Sf 1.19 I pan acid in I pan water). Add 2.5 mL of the
he"achloroplatinic acid solution and milt.
X3.2.4.6 PotQSsillm}odatt. Siandard Solwion (0.1 N)DJ}'the crystals of potassium iodate (KlO,) at 180lC fOf I h.
Dissolve 3.510 B or the KJOJ in about 200 mL of water.
transferto a I-L volumetricf1ask,
dilute to volume, and mix.
X3.2.4.1POllUS;U", Iodate. Standard Solution (0.00$
apparatus as shown in Fla. X3.1 aud 8tm 1\ very aende
stream or nitrogenthrouah the sys\em.
.
acid solution to the sample. Assemble the
NOTEXU-A now of about 30 c:m'/min is aatisl'Ktory.Ir Ihe
IImpl!: dissolvosrapidly, Ihe now IbO\lldbe dtcrCNiIdduri8l1the time
hydroaea is freelylibe..ted.
X3.3.7.S Coatinue tho hcatiD8 alld flow "fnitrogen until
the sample is completmy dissolved. then continue for 5 min
(Note X3.6).Separatethe sas deliverytubes(rom the evolution head and remDve the m:civin8 Oaskwith the delivery
tube.
NOT! X3.1-Tb,sol"licJn In die reeeiYin. Oask\~ n:mal" alkalir.e
tbJousho\tt the dissolution period if the hot ~llatt Wll'lplraM'e and tbe
nitroaen now are proporly IdJlIstcd. Additional 8mMClnillcalzillc IlIlf.te
solution may be addld, if 1Iec:essary.but tile IImplf: lihould be c1iIeardeci
If the rcceivlnl solll\loo btcoma acidic: (leA thJn pH '7 by \1St paper).
N)- Transfer2SmL of the0.) N KlO) solutiDntoa SOO-mL
X3.2.7.6 Add I mI. of the starch-Iodide solution and 5
volumetric flaskwith a pipet, dilute to volume,and mix.
X3.2.4.8Starch Solution (10 gIL)-Potassium Iodide (50
mL of diluted HCI (11'I) and mix. Titr-ateImmediately with
.
tlL) Solution-Add
about 5 mL or water to I S of soluble
Standard potassium iodate trom a tO-mL burtt to the first
blue color. Draw some of the soluticln into the delivery tube
wi\h a Nbber bulb and ~lease along the Deckof the na$kto
wash down any adherins zinc sulfide. Swirl tM solution to
wash the O\ltside of the tube. Continue the titration to a
permanent blue color.
X3.2.1.7 Run a blank titration to the samt $tarch.iodine
coloron a mixtureor 20 mL ot water,3 mI..of ammoniacal
starchwith Stirrinsuntil a paste is (ormed and add to 100
mL Qfboilinawater.Cool. add 5 I Ofpo1asi1iumiodide (.KJ),
.
.
And slir unttl the KI is dissolved.
X3.2.S Sample PrepQralioh-Prepare sample as outlined
in X3.1.7.
X3.2.6 Weight .0/ Sample-Select and weith to the
nearest 0.1 m& an a.mount ofsarnple
E.~r.cd SlIlr"'t Co-nltnl.
I).OOSto 0.07
o.OS 102
maas
.
as follows:
Weiahl
zinCsulfate,I mt of starch-iodatesolutionand 5 mt of
or SIImpir.
I :t 0.02
1.0
diluted h)'drOQhloricacid (1 part UC:Isp sr t.' 9 and 1 p~11
water) in a So..mLli.rlenrn,)'or nask.
0..
X3.2.7 Procedure.X3.2.7.1 Weigh the specified amountof sample to the
nearest 0.1 DIgand transfer to the SO-mLevolution flask.
X3.2.7.2 Add 20 mL of water and 3 mL of ammoniacal
1Ine sulfate solution to the receivina nask
X3.2.7.3 Adjust the hot plate to maintain the temperature
of 2S mL of waterin I SO-mLErlenmeyer
RISkat 80.C.
X3.2.8Caiculation.s-CaJoulate
the masspercent of sul-
fide sulfuf as foUo\Vs:
I" mau t!l
. SUllid
I ~su,ur,
JV.
where:
(.4
-B
)(
0.005~ 0.016) X 100
W
A. = 0.005 N KIO) solution used for the sample titration,
.
mL,
B - 0.005N KJO,solutionusedin theblank,mL,and
X3.2.7.4Add IS mL of the hydrochloric acid.
~:
W
- sample used, I.
x.. DETERMINING TH;E NUMBER OF DJSCON11NUmES IN CHROMIUM ELECT.ROPf..ATING
.
(DUBPERNELL TEST)
X4.1 Pri","iplea/the Me/hadl-Copper will be deposited
on nick.elexpDsedthrouGh discontinuities in chromium but
,--
anodic votta,e or tilne becausenickc:1will slowly di&solveor
become passivated.)
Bath formulatioD-(Don.mdca1)
. not on the chromium,providedthat potentialis properly.
controlled (kepi Jowenoush to avoid activation of passive
CuSO,.5H2O i UI (250&,L)
H2SO, (Spa 1.95) 0.5 m (20-2S.C)
chromium).
Temperature
(rO(lm)
X4.2 Prepo.rllliol'lolitsl Pitel:
X4.2.1 Ma$k all edaes not co\lered by the chromium with
Anode (copper)
a nonconduclive paint or preS$uresensitive tape, includins
Uveentry
.
the wire used to make contact to the calhode bar. After
X4.2.3 Following copper electroplating, carel"uJJyremo\'e
the specimen, rinse in cold then hot deionizl:d wa~er.and air
masking, clean the speciqlen by sOlkins in a hot alkaline
cleaner until the surface Is free or water breaks. A mild
dry. The specimen should nOI be wiped where pores or
cracks aM to bt counted, nor should the part be force air
sCNbbin, with I 50n brush is helpful. Follow the c:1caninaby
a thorou&hrinse in cold deionized wIter, then a dip in a 5 "
dried. Drying can be AI:celeratedby ro1lowinSthe last water
by ma$Ssolutionof H2SO".
.
rinse by a rinse with aJcohol (ethanol) or other vDlatilewater
miscib)e solvent.
X4.2.2 Make freshly cl~.I\C<isample anodic at 0.8V for 30
s in the copper plating ba\h, then switch to cathodic (see Fia.
X4.2.4 Tbt copper deposits only on the ullderlyinsnickel
X4.1) 8t appr~ximately 0.2 to O.4V. for 2 min (see Notes
that is exposed through discontinuities (pgR'.Jiand cracks) in
the chromium.
X4.J and X4.2.);'CCautJon-Do nOI &0beyond the specified
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X4.3 Asse.ssmenl:
X4.3.1 The numberor discontinuities
in tho chromium
can be estimatedby countingthe:coppcr nodules
deposited
within a known area of the specimen or the number of cracka
In a known leftlth. These determinations are facilitated with
a sncta11\lllical
microscopefitted with a calibrated",ticle in
the eyepiece,Ot from
1 J'i"-'.
O='.::
.L.L;J;;J
I',W. J.QQ
nuJ.J.'
X4.4 Dwl.rmlnGlion of Acllve COIrQJionSit's By Corro-
sionTesling: .
X4.4.1 Before\estin& the part shoulci bq,cleanedto
eliminate wacer breaks. Mqneslum oxide. warm water and
soap, or solvents, or 8 combinat.ion therel)l~ tJ\iSht be
necessary
for thorau&h cleaniu8.
X4.4.2To developthe ac;tive corrosion sitcm~subject the
part to the number of houn of CASS exposure corre--
pbotomicrosraphstaken of a ",presen-
spondln8 to the corrosion spedfication for tho required
service condition And thickness specification. After CASS
lestin,.ril15ethe part in warm waterto removeIhe saltlayer.
If the part contains corrosive product scaininn,it can be
washed with a very mild sponge in warm waterbut the paR
should not be. subjected 10 an)' abrasivecleaning. After
dryint either by hot air or solvent suchas n~ethanol.the pan
should be examined at a masnificAtion between 100 and
2001. and the active pan: size Dnd densitydetermined.The
conadin, pore sites are typically distinctly latger than the
unconodcd sites Ind havea darker and roushertexture. By
means of photosraphsat I 'known magnification,the active
pore site$ can be counted and the "cUVt $it-CI.per Irea
calculated. Different photographs should be taken at the
same magnificationat all significantsurfacesand cunent
densities to recordthe ditrerencesin pore density and size
Nora X4.t-b8le1 potentia).usedI, dependallton ancde~thcde
spacing.At IIdiS\anc:eof 8 10 10em. 0.2 V usuallyproducestho desiRd
deposit. As ,pacinI incroaK'S.th. poI.ntlal can be Incl'O8$Od
100.4 V.
NOT!!X4.2-Aner cleani"s. anodle rreatmellt to tepat.sivatt:chro-
after corrosion. As a auide, the: averaac dJanleter orthe active
sites should not exceed0,032 mm (0.00125 in.) and the
largest individual site should not exc«d 0.063Smm (0.0025
miumIs essential.Platinatlm. cainbe varied(rom' to S min.Two
min1lteshASbeen found to he near optilnum.With hisht)' porous
in.).Comparisons
with krJownpore density chans can be
usedfor determination
orthesiteSpersquarecenthnetre.
lonser times illeur risk Qr merlina the deposit nodules,
&ivln.rift to ambiluitin in cauntllli pores(nodules).
X4.4.3 Even thouah the nec:essary work has not been
conductedto estabUsha correlation betweenactivecorrosion
sitesand stanina aiteles measuredby DubpemeU. it appean
that for a givencurrentdensityand depositsystemthereis a
comlation between the number of poresbefor~corrosion
andthenumberor active corrosion sites anerCASStestina.
Once this corrtlation he been established
at a giveninstal.
lation, a simple 100 to 200 X viewina or a pan misht
X4.3.3 PrecQul/(ms-Do not exceed 0.6 V cathodic. High
cathodic potentials CAnactivat~ chromium loaIUy,8ivins risc
to spuriously his.hnodulecounu. If this condition is suspected, it can be tested by gently wiping the copper ofl'wlth a
..tissue. If copper adbe:m to specimen; it is probable the
cathodic potential was too hlah. tbus depositina copper on
the chromium instead or just i.- tho pores.
~
~
1
R,
e~.
A
V-SOURCE
R.:
E~
c
A3
e
EA- 2-1
.
.
.
Fla. X4.1 Schamlltle DI
.
.
s 1 DPDr switCI'l
posilion 1 . cathodic
+ As
A, R, ... R3
Ec.
pasltlan 2
Rs
R +R + R
. ~
. anodic
NOT!: Ammeterand voltmcuercan
tie replacedbya 2 ChannelSlr1p
chart recorder.
.
o. . 8"10111"8App.,.tua t6 ConvenlenllyCe/ltl'OIPOltlrltr81111
Volta;. DUrI,,-Para.l" T.8t1nllVIIeo,ptt
O,poIlUOft
10
Et'd
"'.I.'
B 45&
tative field of the specimen. (See X4.4 for a pide to the.
detennination ot active: cOn'Osionsites in the chromium
layer.)
.
X4.3.2 Current measuredor recorded durina the cathodic
cycle,or both. servesas a reliableindi~tor of porosity,[(
current remains low «I mA/cm2) durina the cathodic cycle,
porosilY is low. Rapidly risins cumnt (6//41 = I to 2
mA/mln) and hip (2 to 4 mA/cm2) final current is
iddicati\'c of high porosity. Use of a strip chan recorder
provides a pennanent record of the test current. With
experience, direct counts of nodules of Cu deposited can be
reduced to periodic verifications as the f.r silDature. A
qualitative visual check (microscopically) will then sufficefor
re,loIlarroutine use.
. chromiuM.
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1456
the thicknessand potentialsor the d~J)ositIystem.and the
desired trade-off betwetenbasis metal corrosion and stainin,
in CASSo
nond~tructiveJy indicate the service perfonnance of the pan
after carTasian. The desired number of active corrosion sites
has not been definitely established. This number depends
somewhaton the sizeof the poresbeforeandaftercorrosion.
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:md Matori<ltE(ASTM).1916 RaCI!Streel,
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