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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.ctroplateds 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; ,1 A5"1'M$I...IIII.,dy.VOl0).02.

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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',

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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

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cUo."".."

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MICSGllilllllihaalJllU')

>0." 11'1""

TOil"'1

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1D':'28 "

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01 NIC'l8I

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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 surrhall 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 dQlit(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

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07/19/95

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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 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.

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Ia::' ; =>~

t:.1't\:lJ r~t:.t:.r::I 1"11.;:1 '_U.,

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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 dosll$011thc more ac:c:essIble Specialricks mlY Involvc~hcU5Cor conrolTltlng.aUliiliary.or bipolar eleeU'Odes or ft
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 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!Ic1rl8brlQ ,""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.resent 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:
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 rel="nofollow">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 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 Prar~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 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 i'iate the test 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 X3.1.1.3Coattbeivated Ie$! '\lith 25 to 37J1m . Practices E 50 (Apparatus No. 13). or nickel deposited from the same soluda" using tbe same X3.I.S Reagenl$: . . 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 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. - .

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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 t. A washbottle fitting with a No. t 9/38 inner t ~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.

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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 ivated.)

Bath formulatioD-(Don.mdca1) . not on the chromium,providedthat potentialis properly. controlled (kepi Jowenoush to avoid activation of ive 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 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
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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.

~

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Fla. X4.1 Schamlltle DI

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s 1 DPDr switCI'l posilion 1 . cathodic

+ As

A, R, ... R3 Ec.

pasltlan 2

Rs

R +R + R . ~

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NOT!: Ammeterand voltmcuercan tie replacedbya 2 ChannelSlr1p

chart recorder.

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o. . 8"10111"8App.,.tua t6 ConvenlenllyCe/ltl'OIPOltlrltr81111 Volta;. DUrI,,-Para.l" T.8t1nllVIIeo,ptt O,poIlUOft

10 Et'd

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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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