ML20116F545

Intervenor Exhibit I-165,consisting of Undated Code Ansi/ ASTM a 262-77a, Std Recommended Practices for Detecting Susceptibility to Intergranular Attack in Stainless Steels

ML20116F545
Person / Time
Site:	Catawba
Issue date:	10/11/1984
From:	AMERICAN NATIONAL STANDARDS INSTITUTE, AMERICAN SOCIETY FOR TESTING & MATERIALS
To:
References
OL-I-165, NUDOCS 8505010128
Download: ML20116F545 (28)

Text

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ANSI / ASTM A 262 - 77a es. *-

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E DETECTING SUSCEPTIBILITY TO INTERGRANULAR Y8 ts ATTACK IN STAINLESS STEELS' A

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[13 The osabe acid etch test 11 These recom mended practrees cover ' rnethod of idemnync. bsn a r pid a

&c foHew:rg fue rests simple e:ch:re.

l those specimem of certain uamieu steef i : 1 Fwnce I

4 - Osahc Acid E1ch Teul tr ClawfNanon of Etch Structures of Stain.i grades whah are essennalk free of suscepn-tess 5teek r %ect:ons 2 to 6. mclh Nb to intergrandar anan awoaated *nn N

E chromium carNde prearnates i 1: Fwru e B - Fernc These spect-t Ud Teu for derecnne wssernNhts to mrer. Sulfate sulfuncj Tem w th hJs e lo*

CoMNn rates i,.ena:n C """"" "' d n d *' f' k f' creu!ar anack m stamleu veek (see $cenorsnated Iscreened) hom teump as._ 3ce r_'a; _

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14 The fernt wuate%nu is aad teu the

.rc vcernNhn m ir ergrarwr anad m

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t see Nee mn 14 to :l' mdi aad reu are 5ased on *ep b 2erma-a!%

D - N a ric-H s droiluoric no s and. thus ie k J Teu Wr Je'echre su cernNh's lo in'er pros tde a Quar utatn e mea.

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wre o e relanse pe@rmme of speccens

, Nar anack m wh hdenum.beanne aus-esalaa ed in cemrau. the copper-correr s l-l nx cam:ess ueek nee secnons, :1 io :-

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,' d and ual enamo nanon of bend Teamens ard. rherefore daw

!15 Pra ru e E - Copper Copper Sulfate-u res the speamem onh as accerraNe or non-Uanc Acid Tes: for derecong suscernNhn d "'I'd N'

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tercranular attack m udmlew ueek (see I'"

kmonjs, O'pper sulfate wlfunc aad teu et i: The foHowmc f actors cosern the apph-I' f"C ""# ' '"U ""C 3 the. D h d" '" % I' d * h hr of these rewmmended prachces

'ne esahc aad etch teu *in prouce the re-

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': 1 SuscernNhn to intercranular anni ped mimanor 1r the shonest 8'" c;df ed *1f h the preClpliai r re AM of chromidm P

edes is readih de'ec'ed ir au f n e tem Id #

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h senting as nearly as pomble the w hich represent steelintended for use in mtric 2.3 The grades of stainlew slech and the matenal a'it *'ll be used m scru acid environments.

hot acid tests for which the omahc acid cich surface finishing should be pei j

l.6 For AISI Grades 316.316L.317 and test is applicable are listed in Table 2.

,cquired to remove foreign mai 6

317L only, the nitric-hydrofluoric acid test 2.4 Extra low carbon grades,such as 304L. ' tain a standard, uniform finish a i W may be used to provide test results in 4 h.

316L. and 317L. are tested after sensiiizing 4 3. For very heavy scciion

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1.7 The 24tkh nitric acid test must be ap-heat treatments at 1200 to 1250*F (650 to should be machined to represc 1

se plied to stabilized and molybdenum-bearing 675*C) which is the range of maximum car-pnate surface while mame.nnir grades intended for service in nitric acid and bide precipitation. These sensitizing treat.

specimen siec for convenient les to all stainless steel grades which might be ments must be applied before the specimens ih. remosal of more matenal 0 subject to end gram corrosion in meric acid are submitted to the oxalic acid eich test. The will hase little influence on the F*

service.

most commonly used sensitizing trealment is 1 Howeser, in the special case o 1.8 Only those stainless steel grades are h at 1:50*F.

bunzation (sometimes encount listed in Table I for which data on the applica-stance m tubmg or castmgs *t tion of the oxalic acid each test and on their

3. Apparatus or binders containmg carbonace y-performance in various quantitative esalua.

3.1 Source of Direct Current - Batter).

are employedi it may be pow tion tests are asailable.

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1.9 Extensise test results on sarious types about 15 V and 20 A.

the carbunzed surface. Such tre.

generator, or rectifier capable of supplying gnnding or machinmg to compi of stainless steels esaluated by these practices 3.2 Ammercr-Range O to 30 A (Note 1).

specimens is not permnsible, e have been published m Ref (10).2 3.3 Variable Reststance (Note 1).

undertaken to demonstrate suct 3.4 Ccihode-A cylindrical piece of stain-4.3 Pohshing-On all types FO A SIF AT NO ETCt Tt C.

less steel or preferably, a 1-qt (0.946-litre) cross sectional surfaces should b

} *F TURES OF STAINLESS STEEL.S (1) stainless steel beaker.

etching and microscopica exami 59

2. Scope 3.5 Large Electric Clamp-To hold speci-imens containing welds should i

h 2.1 The oxalic acid etch test is used for plate, weid heat-affected men to be etched.

zon

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acceptance of matenal but not for rejection of 3.6 Aferallurgical Aficroscope-For exami-metal. Scale should be remos ed p

matenal. This may be used in connection with nation of etched microstructures at 2501o 500 to be etched by gnnding to an i diameters.

other evaluation tests to provide a rapid fimsh on a gnnding belt or u method for identifying those specimens which 3.7 Electrodes of the Eiching Cell-The excessive heating, and then poli are certam to be free of susceptibility to rapid specimen to be etched is made the anode, and cessnely finer emery papers. N miergranular attack in these other tests. Such a stainless steel beaker or a piece of stainless

%. and %. or finer. This poksh i specimens hase low corrosion rates m the var-steel as large as the specimen to be etched is can be carned out m a relaine ;

made the cathode, since all large scratches need not y;

ious hot acid tests. requinng from 4 to 240 h 3.8 Electro /vic-Oxalic acid. (H:C.Oc

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of exposure. These specimens are identified

. heneser practical. a polished W

i by means of their etch structures which are 2H:0). reagent grade.10 weight G solution.

or more is desirable if any ci e

I classified accordmg to the followmg cntena:

Non 1-The vanable resistance and the amme-dimension is less than I cm.

1 2.2 The oxalic acid eich test mas be used to ter are placed in the circuit to measure and control length of I cm should be polish.

j screen specimens intended for testmg in Prac-

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"'h' 'P"'**"'* D*h'd' asailable length is less than I cr section should be used.

B-Ferric Sulfaie-Sulfuric Acid Test.

tice h

Practice C-Niinc Acid Test. Practice D-

4. Preparation of Test Specimens 4.4 Eiching Solution-The -

for etching is prepared by add 4

Niine-Hydrofluoric Acid Test, and Practice 4.1 Curring-Sawing is preferred to shear-reagent grade oxahe acid crys:

C E-Copper-Copper Sulfate Sulfuric Acid ing especially on the extra-low carbon grades.

ll$O) to 900 ml of distilled wat:

Test.

Sheanng cold works adjacent metal and af-1 until all crsstals are dissobed.

2.2.1 Each recommended practice con.

fects the response to subsequent sensitization.

4.5 Erc5ing Conditions -T tains a table showing which classifications of Microscopic examination of an etch made on a s

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etch structures on a given stainless steel grade specimen containing sheared edges should be mm. To obtam the correct curre specimen should be etched at 1.

are equivalent to acceptable, or possibly non-made on metal unaffected b sheanng. A con-4 5.1 The totalimmersed are.

3 acceptable performance in that particular test.

venient specimen size is I by 1 in. (25 by 25 men to be etched should be I

Specimens having acceptable etch structures mm).

l need not be subjected to the hot acid test.

4.2 The intent is to test a specimen repre-4.5.2 The vanable resistance square centimetres, and Specimens hasmg nonacceptable etch struc-

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tures must be tested in the specified hot acid justed until the ammeter reading solution.

.The boidrace numbers refer io hiersture references !

found si ihe end or these recommended pracites 7

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1 senting as nearly as possible the surface of the stamless steels and the material as it will be used in seruce Only such equal to the total immersed area of the spea-

.ich the otahc aad erch surface ftnnhmg should be performed as is men m square cennmetres hsted m TaNe :

required to remove fore.gn material and ob-4 6 &chmg Precounom on gradet such as 304L.

tam a standard, uniform fmish as described m Etching should be carried out under 461 j

rested af ter sensaame 43 For sery heasy secnont specimens a ventilated hood Gat w hich is rapidly

) 20n to 125WF M50 to should be machmed to represent the appro-esobed at the electrodes with some entrain-

range of maum l hese senurarng treat.

priare surface while mamtamma reasonable ment of osabe acid. is poisonous and irritanng um car-to mucous membranes y

l

! hetore the spet:mers

<pecimen sue for consenre-r resorg Ordmar-46: A y ellow-gree n fdm ts gradually I

h remosal of more mateful than necewary formed on the cathode Tha mcreases the wahc acid e'ch res: The el base htfle mtlue ce on the test results W

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nsnamg 'reatment n i Howeser. m the speual case et surf ace car-resniance of the etchme cell W hen tna oc-p i

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curs, the fdm should be remosed by rmsmg Nraat on i so m e n m e s ercourtered tot m-the mside of the stamless steel beaker (or the

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l wnte. in tubmg or castmgs when lubricants Currem - Hauery.

er Smders corrammg carbonaceous materials steel used as the cathode) with an aad such as j

30 c'c H N O:

m are employ edi it may be possible by heavy capanle of supph mg pndmg or machming to completely remose 4 6 3 The temperature of the etchmg solu-i the carburized surface Such treatment of test tion gradualh increases Jurmg etching The eO to M A (Note 1) i speemens is not temperature should be kept below $0'C by i

ce INote 11 permissible, escept m tests ndr: cal pie;e of stam-Wertaken to demonstrare such effects alternanng two beakers One mas be cooied I

4 3 Polishmg-On all types of materols m tap *ater while the other is used for etch-craw secner.al surfaces should be pohshed for mg The rate of heatmg depends on the total

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4 i curre nt (ammeter reading) passmg through e'chmg and microscopical esammanon Spec-the cell Therefore, the area etched should be emp - To hoid specs cens contammg

• elds should mclude base kept as small as possible while at I

rire. w eld beat atfected zone, and weld the same

'm mre - Fo r e s a m e metal Scale should be remosed from the area time meermg the requirements of desiraHe actures at 2 %) to $4iG mmimum area to be etched to *e etched. bs grmumg to an 50 or 120 grit Immersion of the clamp holdmg the k

464 fMh on a grmdmg belt or wheel wahout u

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"ade me r de. and etcessne hearmg. and then polahmg on suc-specimen m the erchmg solunon should be asorded e%eb tmer emers papers. No

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and or tmer ihn pohshmg operanon 4 ? Rmsme-Followmg etchme the 3 pea-a pm c t't na m ess men to ht eveJ w can be carr:eJ out m a relatneh short ome men should be thoroughly rinsed in hot *ater smcc all farve scra:ches need not be remosed and m acetone or alcohol to avoid crystalhza-

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( l4 a6 M e il C 0,

%'ereser practical, a pohshed area of I cm-tion of osahc ac:d on the etched surface dur-mg drsmg 9

weet E soi o nen er more n devraHe if any crow sectional l

4 8 On some speamens conrammg moh b-

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Mewon n few than I cm. a mmimum denum t A!SI 316 316L. 317 317L) which aj ey of I cm should be pohshed W hen the ea e I

J'JdaNe leneth a few than I cm. a f ull crou are free of chromium carbide sewtaation. it a be eer j

\\echen should be used may be difficult to rescal the presence of step structures bv electrohtic etchme *rth otahc mmens 44 &chme Solunon - The solunon used acid in such caset an electrohle of a 10 "c TI

,e r

' referred to shear.

etchmg n prepared by addmg 100 g of solunon of Jmmomum persulfd!e. ( N Has O..

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reJcent craJe osahc aaJ crsstals (H;C O.

l ow carNo er des a

g g,,g m m mas be used m place or osahe aad An erch

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ml of dantleJ a.ocr and stirrmd of $ or 10 mm at 1 4cm m a solurton at

nt metd md d'

"hl all l

.cn r sc%raanon rutak are Jnsobed Y

45 &

room temperature reaJih deselops step struc in em m ue on a m - T he polnhed tures on such speam s

ens edecs sho r

udse

%n she.irm \\som To obtam the correa current dene

5. Cimification of Etch Structures g';

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'2 h 2' g

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to be etcheJ should be measured n

%Jte centirretres, and metallurgical microscope at 2 5i' = f o f Wi = for

'Ph M ' re;'rc-4 5 2 The variable remtance should be ad-arought stech ard at about fo= for cast e

steels s,, -

M'ed untd the ammeter readme m amperes n 5: The etched crowsetnonal areas should

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p 4 l*rm tu r y n a 4 h tes be thoroughly cxammed by compicie trascrse detected by pronounced disches from inside to outside diameters of rods and 5.5 Some wrought spvcimens. especiall) !

acid and 3 % hs tubes. from face to face on plates and acrow from bar stock, may contam a random patternI appheaNe ont all zones such as weld rncial, weld-affected of pits.11 these pin are sharp and so deep' grades of auuen I

316L. 317. 317 zones and base plates on specimens comain-that they appear black (Fig. 7) it is powbie that the specimen may be susceptible to end.

biht) to intergr ing welds, grain attack in mtric acid only. Therefore,i chromium carb-5.3 The etch structures are clawified into the following types (Noic 2):

esen though the grain boundaries all hase detect susceptib 5.3.1 Step Structure (Fig.11-Sicps onl>

uep structures. specimens haung as much or sociated with sy between grains, no ditches at grain bound-more end grain pitting than that shown in sion. w hich. so t Fig. 7 cannot be safely awumed to hase low intergranular at aries.

5.3.2 Dual Structure (F,g. 21-Some nitric acid rates and should be subjected to enuronments ditches at grain boundaries in addition to the miric acid test wheneser it is specified.

6 5 Prachte r

steps, but no single grain completely sur-Such sharp, deep pits should not be confused sdfuric Acid 7 with the shallow pits shown in Figs I and 6 solution contai rounded b) ditches.

c* corrcr si.

sc 5.3.3 Dutch Structure IFig. 31-One or embedded m n more grains completely surrounded b)

6. Use of Etch Structure Clawifications inp. which dett ditches.

5.3.4 Isolated Ferrrre (Fig. 4)-Observed 6.1 The use of these classifications depends ular attack mo in castings and welds. Steps between austenite on the hot acid corrosion test for which stain-chromium-rich matrix and ferrite pooh _

less steel specimens are being screened b) susce ptibiht3 14 5.3.5 Interdendratic Driches (Fig. 5)- Ob-etching in oxalic acid and is described in each ated with sigma served in castings and welds. Deep intercon-of the recommended practices, important both of uhich h characteristics of each of these tests are de-in certain nitric nected ditches.

5.3.6 End Grain Pitting I (Fig. W-ltruc-scribed below.

PR ACTICE I ture contains a few deep end-grain pits a'ong 6.2 Practice B - Ferric Sulfare. Sulfuric FURIC ACID with some shallow etch pits at 500 ~. (Of Acid Test is a 120-h test m boihng 50 "c CEPTIBILITS TACH 1% ST importance only when nitric acid test is used.)

solution which detects susceptibility to inter-5.3.7 End-Grain Piiring II (Fig. 7)- Struc-granular attack associated primaril) with 3

ture contains numerous, deep end-grain pits chromium carbide precipitate. It does not 7.1 This ret at $00x. (Ofimportance only when nitric acid detect susceptibility associated with sigma the procedure !

phase in chromium-nickel-molybdenum stain.

h ferric sulfate test is used.)

less steels (316. 316L. 317, 317L) which is Nou 2-All photomicrographs were made with known to lead to rapid miergranular attack

3) which meas specimens that were etched under standard condi-onh m certain nitric acid enuronments. It less steels to i tiont 10 9 oxabc acid. room temperature 1.5 min ence or absenc at 1 Alcm:

does not detect susceptibihty to end gram test ts not nec 5.4 The evaluation of etch structures con-attack which is also found onh in certain formance of 1 taimng steps only and of those showing grains nitric acid ensironments. The ferric sulfate-enstronments completely surrounded by ditches in ever) sulfuric acid test does rescal suscepitbihty basis for predi field can be carried out relativel> rapidly. In associated with a sicma-hke phase constituent rosion other t cases which appear to be dual structures.

in stabilized stainless steels. AISI 321 and eral corrosio-more extensive examination is required to de-

347, termine if there are any grains completely 6.3 Practice C-Nstric Acid Test is a 240-h crackmc encircled. If an encircled grain is found, the test in boiling. 65 9 mtric acid which detects son.t _ se most appropria steel should be evaluated as a ditch structure.

susceptibihts to rapid intergranular attack as-Areas near surfaces should be exammed for sociated with chromium carbide precipitate and with sigma-like phase precipitate. The evidence of surface carburization.

7.1.1 The 5.4.1 On stainless steel castmgs (also on latter may be formed m molybdenum bearmg ;

detects susee weld metal) the steps between grams formed and in stabihzed grades of austemtic stamless associated wi by electrolytic oxalic acid etchmg tend to be steels and may or may not be visible m the carbides m tess prominent than those on wrought matert-microstructure. This test also reveals suscepti-t steels. It doe als, or are entirely absent. Howeser, any sus-bihty to end grain aitack in all grades of stam.

ceptibility to intergranular attack is readily less steels.

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6 4 Practice D-Naric H drof7uoric Acid tergranular attack associated wuh sigma phase i

3 nced duches Test is a 4-h test in a solution of 10 C*c nitric in austenitic stainless steels containing molyb-3 ght speamens. espeaalk acid and 3 c*c hydro 0uoric acid at 70*C 11 is denum, such as Types 316, 316L. 311 and

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. contain a random pattern applicable only to moly bde num-be arin g 317L.

g is are sharp and so Jeep grades of austenitic stainless steels ( AIS! 316.

Non 4-To J tect suscepnNhn to imergranu-f p

ack (Fig ?) a is posuble 31el. 317. 317L) and detects only suscepti-lar aitack associa.ed wien snima pnase in auuenaic r

uainku unk containing wWenum. o,e nunc nay be suscepnble to end bility to intergranular attack associated with acid test. Practice C. snoulJ 5e used

~i ric aad onk Thererere chromium carbide precipitates it does not 3

7 2 In stabihzed stainless stee!. Type 321

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. rain boundar es all have detect susceptibihts to intergranular attack as.

fand perhaps 347) the terric sultatemalfuric 3

i amens hamg as much or soaateJ with s:gma phase or end grain corro-aad test deteca suscepnbdin anocated anh j

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sion, which so f ar. are known to feaJ to rapiJ itfire than that Oown in preopuated chromium carb des and with a itch issur ej to hD e lo*

mtergranular attack only in certain mira aad

i' d Ih*C

• h'ch me be insi W e in the

.e iJ GodJ t'e subicaed to ens tron meats rmc ros t ruc t ure wheneser a n,pec:heJ

^2 Prxnce E - Coppen Correr bi9:e.

' 3 The terric sultatenult anc aad test mn its shodd rer t,e conf used bl%r:c Acal Ten is a 24-h test in a boihne be used to esaluate the heat treatment ac 3

e "f/

a shown m Fres Iand^

solutio n contamine 16 "c sulf unc aad and f

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corded as-receised material it mn also be

^c copper suHate with the test speamen c

used to check the effectiveness of stabihzing embedded m metadic copper shot or gnnd-columbium or titanium additions and of re-g utture C!nuncation, ings, which Jetects suscepobility to intergran-ducnons in carbon content in presenting sus-

'ese classifwanons depends ular attack assoaated with the preapitanon of rouon f eu Mr 4 hgh vain-chromium-nch carbides it does not detect cepubihty to rapid intergranular attack lt

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may be apphed to wrought products (incluJ-n are heme screened bs suscepubehts to intergranular attack associ-ing nabest castings, and weld metal l rd and n describeJ in eJch ated with sigma phne. or end-gram corrosion.

7 4 Specimens of estra low carbon and sta-t j Jed prastaes Important both of which hase been otssersed to date onk bihzed grades are tested af ter sensit: zing heat

(.

ach of these feus are de-m certain nitric aad ensironments 4

treatments at 1200 to 125WF K50 to n?5'C),

- Te r ric Not w e-h pt'r".

PR \\CTICE B - F E R RIC SL L F -% T E 5L L-which is the range of maumum carbide pre-M w

FL RIC %CID TE5T FOR DETECTING 5Ls-ich test m Nuhne 91 CEPIIBilli) TO IN TE RGR sNL L AR \\ T.

apnarron The length of time of heat:ng used p

ca suscernNhn to mrer-T Rh IN si stNLE55 $ TEEL 5 m for this sensitizing treatment Jetermires the g

i maumum permnsibie corrosion rate for such N

s sou a:c a premanh aan

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E SCOP' grades in the ferne sultate suitunc aad test prear.ve it does nin

'1 Thn recemmended practne desenbes The most commonh useJ sensinzing treat-s Jm sued *dh ucma l me! moh haenu, st am me procedure for conduchre the bothne.12n-ment is I h at 1250 F

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5 ternc sultate-50 "c sulfuric acid testlNote L Rapid Screening Test

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y PL. T I ' it 'Li w ngh is rapid imercrandar attad h w hich measures the suscepnbihty of stain-

'nc aad enuronmenn ir ten steek to intergranular attack The pres-41 Before testmg in the fernc sulfate sui acePhNhh to end gram ence or absence of mrergranular attack m this func aad test speamens of certain grades of r

'eM is not necessanly a measure of the per-stainless steels (see Table 31 me be gnen a No founJ onh m certain ments The terne sult ue.

tormance of the matenal in other corrosne rapid screemng test in accordance woh proce-Joes resca suscernNhn emironmenn The test does not prouJe a dures gnen m PractNe A. Osahc Ac:d Erch 5

Tesi for Clasuficanon of Etch structures of cmaMc Mne sonsotuent

% for preJKring resntance to forms of cor-w s:ce's TISI 121 and twon other than intergranular, such as gen.

Stamfess Stech Preparation. etchmg. and the clasufKation of etch structures are desenbed g

eral cor rouon, pit t i n g or st rew-c o r ro3.o n therein The ne of eten structure es aiuanons

\\aN bei leu n i 2 4+ L h crJdmg in connection with 'he terric Mrate-suMunc

)

nuts as tJ w h N h Je tec

%E 3 - M Prw \\ W re unon on t he Jad !csf a st'eaneJ m Tarie 3 d inh rerandar aitak 3 mou y,propnje at twe ses er al 'eu meMmds mda-

1. f h *' J i"J ' "' "I 'IC' h' s t ad e s o f " J o c "

4 1 1 Corros.on test s pe u m e n s ho me ac.

mum carNde preurna'e veet ceptable etch structures in the osabe aad etch i

J m n% Nk numhearme II The terne sulf ate 4ulf ur c aad test test will be ewennaih tree of intergrarular l Ed 5

phec prnirnaic 1 hc ides or auuc nh u amled Je'eca suwe;'nNhts to mtergranular attacs attack in the ferric sulfate-sulf urn aadteu

{. '

na ut he s n.He m the aNctated woh *he preapitation of chromium Such speamens are acceptable without res*mg I

hu ao re s cah suw e pt,.

CarNJes m unuaNh/ed auuenitN uamiew m the ferric sultatenuif ur;c aad test AN gec

&, (W[. ;

e f as k m dl grades or u im.

Meeh lt doeg not detcct suggptiNjits to in-imens he mg nonaGeptatdc e!ch uruciares y; DC

[9 'N M I"w s

_WW

,J M...

v J.

~

ye

-y

(

l t

h A 262 l

must be tested in the ferne sulfate-sulfuric Erlenmeyer flask.

11.4 All surfaces I

acid test.

10.1.3 Then measure 236.0 mi of reagent in edges. should be grade sulfuric acid of a concentration which abr.i w pa must be in the range of 95 0 to 98.0 % byf used, poinh slow

9. Apparatus 9.1 The apparatus (Note 6)is illustrated in weight in a 250-mi graduate. Add the acid, s' and blaump shoul.

i Fig.8.

slowly to the water in the Erlenmeyer flask so.

113 All traco o I

9.1.1 A four-bulb Alhhn or Soxhlet con-avoid boiling by the heat evolved.

ing heat treatment.

denser with a 45/50 ground glass jomt. Over-Norn 7-Loss of vapor resuhs in concentra" "

mosed Any wale '

i of the acid.

alllength: about 13 m. (330 mm), condensing gnndmg, for es s

section 9% in. (241 mm)-

10.1.4 Weigh 25 g of reagent grade ferne hers. muu be remos 9.1.2 A one-htre Erlenmeyer nask with a sulfate (contains about 75 c'c FedSO.)3) and' imen m concentra 45/50 ground glass joint. The g*ound glass add to the sulfunc acid solution. A inp hal-

oWF (9.VC) (Re opening is somewhat over 1% m. (38 mm) ance may be used gah an c action anc wide-10.1.5 Drop boiling chips into the Oask-the test solunon )

9.13 The glass cradle (Note 5) can be suP-10.1.6 Lubricate ground glass jomt with 116 The specim phed by a glass-blowing shop. To pass through silicone grease ciudmg the mner su the ground glass jomt on the Erlenmeyer 10.1.7 Cover flask with condenser and cir,

voial exposed area flask, the width of the cradle should not ex-culate coohng water.

11.7 The specir J

cced 1% in., and the front-to-back distance 10.1.8 Boil solution until all ferne sulfate greased and dned I

I must be such that the cradle will fit the 1%-in-is dissobed (see Note 7)-

naied acents such then we'ighed to th (34-mm) diameter opening. It should hase three or four holes to increase circulation of

11. Preparation of Test Specimens the testing solution around the specimen.

11.1 A spectmen havmg a total surface

12. Procedure Norr 5-Other equnalent means of specimen area of 5 to 20 cm: is recommended. Speci-1; i piace speci support.such as glass hooks or siirrups. may also be mens containing welds should be cut so that metse in boilme so used no more than %-in. (13-mm) width of base.

12.2 Mark 15 qui 9.1.4 Boiling chips must be used to present metalisincluded on either side of the weld.

crayon to proude a bumpshg.

11.2 The intent is to test a specimen repre-would result m co-3 is recommended sentmg as nearly as possible the surface of the ;

there is an apprecia 9.1.5 A sibcone grease for the ground glass jomt.

matenal as used in service. Only such surface test must be repeai 9.16 Dunng testmg, there is some deposi-finishmg should be performed as is required to.

recround specimen tion of iron oudes on the upper part of the remose foreign material and obtam a stan-12.3 Contmue i Erlenmeyer flask. This can be readily re-dard, umform fmish as specified. For ser) for a total of 1 0 mosed. after test completion, by boihng a heavy sections, specimens should be m a-rinse in water and solunon of 10 c'c hydrochloric acid m the chined to represent the appropriate surface '

12.4 Weigh spe flask.

whde mamtaining reasonable specimen size !

from ongmal weic 9.1 7 A device such as an electricall) for convenience in testing. Ordinarily, re-l 12.5 No mterrr heated hot plate which provides heat for con-moral of more material than necessary will.

alh necessars. Th tinuous boihng of the solution.

have little mfluence on the test results. Ho*- l mterrupuon 'for 1-91.8 An analy tical balance capable of eser, in the special case of surface carbunza '

nary results are de weighing to the nearest 0 001 g.

tion (sometimes encountered, for mstance,in l remosed at any tir Nort 6-No substitutions for this equipment tubing or castmgs when lubncants or binder 5 I 12.6 No change mas be used The cold-hnger type of condenser contaming carbonaceous matenals are em-I during the 1 0-h t with siandard Erlenmeyer flasks may not be used ployed) it may be possible by heasy gnndmg 12.7 Addinonal l

l

10. Ferrie Sulfate Sulfuric Acid Test Solution or machming to remose the carbunzed layer hase to be added i 10.1 Six hundred mdhhtres of 50 '~c (49.4 completely Such treatment of test specimens sion rate is estrao s not permissible. escept in tests undertaken by a change in the to 50.9 ("c) solution are to be prepared as to demonstrate such surface effects.

ferric sulfate must go;;o g 11.3 When specimens are cut by shcanng.

loss of all specime 10.1.1 Caution-Protect the eses and use rubber gloses for handhng acid. PIace the test the sheared edges should be refmished b) test. ferne sulfate i machinmg or gnndmg poor to testmg.

for each I g of dr flask under a hood.

10.1.2 First, measure 400.0 ml of distilled

, Do. cormng sioccock Grease has been found sans-water m a 500-ml graduate and pour mto the factory for this purpose 6

i

i W

=

l J

i i

i 4

D h A 262

) 36 0 ml of reagen-114 All surfaces of the specimen. includ-multaneoush I ncentratior; whicb

- The number (3 or 4)is hmaed 1

U" e

J e

• e

'5 0 to 910 "c by is used, polish slowh to asoid overheating t

Me e acid, Sand blastme should 'not be used

13. Calculation and Report

[

+-

rfenmeser flan tolt 115 All traces of oxide scale formed Jur-13 i The effect of the aad solunon on the 1

i ing heat treatments must be thoroughly re-material sha!! be measured bs determinme the t

Jts in contentrat' r

mosed Ans scale which cannot be removed loss of weight of the speamen The corro'sion I

bs grirdirg. for example in stamped num-rates should be reported as inches or penetr e ieent grade ferru y

1 FeisO u and bers. must be remosed bs immersmg the spec-non per month (Nore 51. catca; ate d as foi-5 imen in concemrated mir:c aad at about lo w s 2non A enp hat

>o'Ft & C) : ReuJual oxide scale causes E.

Innes per w,m h = < y a,a4 ai gahars acam anJ s msequert actn anon m

~

mf" thC dai ihe teu solunon t

gJw pamt with i! 6 The speamen shou!J be measured in-

1. U f # ' I" '# ~ h '

d cluding the mner surfaces of ans holes and the

'I

indenser and ar i l

tool espose) area calculated b '"

11 ' The specimen should then be Je-

'E all fernc suMate greased and dr:ed usmg sunable norchlori-for chromium nickel steefs. J =. 9 g cm) g 4

nated agents. such as soap and acetone and for chromium-rickebmohhdenum weels J=

a then weighed to the nearest 0 H01 g 3 Un g cm 4

1 mens Nort s-Conseruon factors to other comme

• a total surface

12. Procedure a

mended S pe ci-used unas for corrouon rates are n fodo*s h

12 1 t be cut so thar Place specimen in g! ass cradle and im-

'"'"N*"*'I

'"# PI

}*

'"*'N"""**

I - """M P" " "

I width of b ae merse m boilmg solunon incnes per moneh = 12.000 5

mas per scar a

12 2 \\fark liquid les el on flask with was incr es per month = C50 = Jensits = -rdhgra ms

{

p crason to preside a check on sapor low which

' "' P" reamen repte.

in @cs m m nth *M9 wou!J result in corcentrar on of the aaJ If Jenn = cam per

1. '""M "I

• C ware me re ner Sour h sum h surtase there a an appremNe chance m the lesel. the i no in

= $ 45cm; c

test muu he repeated wnh fresh solunon and a s is reared r,

3 obram a stan PR ACTICE C-SIT RIC ACID T F 51 F O R D E-2 a

e T E CTIN G s L SC E P TlHit. li ) TO IN TE R-

,f.

I.

L onnnue :mmers,on of the speamen E."r vers GR O ugR griACA IN STUMFw Mr a total of 1216 h. then remose speamen.

5TEFIs

'ouM be ma.

^

rinse m *ater and acetone and dry I"' ""J" 12 4 Weigh 3peamen and subtract weight IJ S(UPe y

' P'" * ' ' W e 141 Thn recommended practice Jescribes

' p from or emal weight

)rdmarih. re 12 5 No miermediate weighings are usu-the procedure for conducting the boihng nitric necewm wm

h necewars The tests can be run wohout aad test (3) as emplosed to measure the rela-

"Ih HO*-

m'erruptmn for 120 h However, if prehmi-tne suscepobiiny of austenitic stamless week h

ice cathunza

%rs rewits are desired. the specimen can be to intergranular attad The presence or ab-

• '""J""

remosed at ans nme for weighng sence of mtergranular attad in ihn teu n rot

'M or Nrder' 12 h No chJrges in s0lution are necewJrs nece%anh J measure of the pertori"Jrce of

['

O J'c "m-durmg rne 12ibh rest penods the material m other corrous e erwironments.

iI n s ermJme 12 ' -\\JJinonal terne suit.ite mhiNtor mn m parncular, it does not provide a han for iunted !ner hae to be aJJed during the test if the corrn-prcJachrg resniance to forms of corrovon

?

" 'PC # C"'

uon rate n entraordmanh high n es eJen cJ other than mtergranular. sucn as generai cor-h

]

s u rJe r r a ke n N a charge n the color of the solution \\ fore rouon prttmg. or strew-corrouon crackiv

[

h terric sulfate must he aJJed rf the total weight 14 2 The hoehng nitric acid teu mas be i j.

]'s shcanne ow of all speamens etceeJs 2 g (Durmg the uscJ to esaluate the heat treatment accorded

. i

' nnht J %

teu. terne sulfate n conwmed Jr a rate of II' g

'Jv reCen eJ mater:Jl It n Jho somenmes

' (;

'"C for each 1 g of Jmohed stamlew weel )

useJ to check the effectiser'ew of stabih/mg 29 \\Cs CrJI sf'Ccimens mas be tested M-Clemenh dnJ of reJuctions in carNm consent

?

%,r.

l 7

m.,h

[g Q, k.1,[C *.,

e*

=?

,7 w

u.p. m h

I l

• y e n,. L ~

s.

~

b d'~4.

t

• ( -

[

' p3 ' -.

/

]

,s

^

l gYg- + 1 = '-

s5 l

p

?

\\

h A 262 1

in preventing suscep : ilii) to rapid intergran-agreed upon between the surpher and purchaser p, Preparation et j

One of these consists of a one-hire Erlenmeyer flag I

ular attack

• with a ground glass jomt and equipped with a 30-m I81 The m,e Norn 9-intergranc.e attack in nitnc acid is (762-mm) reflux condenser;it has been shown that rnu t be considero associated with one or more of the followmg: (J) results obtained with a reflus condenser tend to be s

intergranular precipitawn of chromium carbides, somewhat higher than with the cold fmger-t>pc con.

(acilitics for accura (2) wgma or transition p ases in molybdenum-bear-denser due to greater vapor loss. The second type of*

o( test solution ti mg grades, and U) c;ma phase constituents in container is the so called multi-sample testing appa..

I staoihzed grades. The tuling nitric acid test should ratus (4) which was designed to permit the testing of maximum conseni l

not be used for extra lom carbon molybdenum-a large number of specimens simultaneously by pr*

about 100 g Sp U

bearmg grades unless the matenal tested is to be viding for replacement of the acid in contact with 5hould be cut so tt j

used in nitric acid serme. See Practice A. Omahc the specimens several times per hour with redsstilled mm) width of base Acid Eichmg Test, for information on the most acid. Because of the lesser accumulation of corro appropnaie of the sesersliest methods available for sion products in the testmg solution, the rates ob-side of the wcld I l

.f' the evaluation of specific grades of stamless steel.

tamed with the multi-sample tester are consistently b.ir. wire, and tut iC lower than those obtamed with the conventional tion of the tota; a j },

14.3 Specimens of extra low carbon and apparatus; the differences are small on property stabilized grades are tested after sensitizing annealed or stabihzed material which will show low posed crou secho' l

3 rates in both types of test but can be very large for Cross sectional art heat treatments at 1200 to 1250*F (650 to 675'C), which is the range of maximum car-5*" fe' esul [ c compaUed d recN), it Ys subject to end gra he bide precipitation. The length of time used for essential that the same type of apparatus be used for proportion of en all tests.

should therefore t' this sensitizing treatment determines tN: max.

imum permissible corrosion rate in the nitric 16.2 Specimen Supports-Glass hooks, face is actually ro t acid test. The most commonly used sensitizing stirrups, or cradles for supporting the speci-ing nitric acid. WP ucts are being te treatment is I h at 1250*F.

mens in the flask fully immersed at all times tions, the ratio of 14.4 This recommended practice may be during the test and so designed that specimens applied to wrought products (including tested in the same container do not come in posed to the tota stant from test to tubes), castings, and weld metal of the various contact with each other.

grades of stainless steel (Note 9).

16.3 Hearcr-A means for heating the test specimens cut fr.

solutions and of keeping them boiling should be propor-the exposed cros?

15. Rap,d Screem,ng Test throughout the test period. An electrically i

half the total espo-15.1 Before testing in the nitric acid test, heated hot plate is satisfactory for this pur.

18.2 Special hi specimens of certain grades of stainless steel

pose, as given in Table 1 may be given a rapid 16.4 Balance-An analytical balance capa-Prior to testing or contain a weld mz screening test in accordance with procedures ble of weighing to at least the nearest 0.001 g.

18.3 When spe given in Practice A. Oxalic Acid Etch Test for Classification of Etch Structures of Stainless

17. Nitric Acid Test Solution the sheared edge Steels. The use of the etch structure evalua-17.1 The test solution shall be 65 : 0.2 machining or gnn IS.4 All surfac tions in connection with the nitric acid test is weight % as nitric acid determined by anal).

specified in Table 4.

sis. This solution may be prepared by adding ing edges, should 15.1.1 Corrosion test specimens having ac-distilled water to concentrated nitric acid (re.

1 0 grit abrasise, is used, polish s agent grade HNO, sp gr 1.42) (Note 11) at ceptable etch structures in the oxalic acid etch 3

test will be essentially free of intergranular the rate of 108 ml of distilled water per litre of Sandblasting sho.

18.5 The inter attack in the nitric acid test; such specimens concentrated nitric acid.

senting as nca@

are acceptable without testing in the nitric Nott Il-The mtric acid used should conform material as it will acid test. All specimens having nonacceptable to the recommended specifications for analytical etch structures must be tested in the nitric acid reagent chemicals of the Amencan Chemical Soca-surface machinir 3

ety 15) as follows:

required to remi test.

Nonvolatile matter, max, %

0.0005 tain a standard t.

16. Apparatus sulfate (SO.), man, %

0.0002 18.4. For ser>

16.1 Container-A 1-litre Erlenmeyer Arsenic, man. %

0.000003 should be machi Chlonne, max. % about 000007 flask equipped with a cold finger-type con-Heavy metals. max, % about lead 0 0005 priate surface w 00001 specimen size fot denser, as illustrated in Fig. 9, is recom-andiron mended.

In addition, the fluonne content shall not exceed dinaril}, remos a 0.0001 % and phosphate (PO.) shall not exceed, essary will hase Note 10-Two other types of containers have been employed m the past and may be used if 0 00002 %.

results. Howevet fa:e carburizatic 8

}

~

y a

y,

.c-: m-

..+

[

.f..

v.

..e A. r

~

r yg y,9QW

,=..,.

s.

R kI A 262 f.

ppher and porc%er 4.-

?

hire E r!e~reser Cau

18. Preparation of T est Specimens for mstree. ;n t uhme s r cau "cs * *en IJri-

's -

qwpre J.oh a h wn O

is 1 N n ar d 3hape of the spec: men C3"lS ' >r he rJers con ta m t r e ca rN ma s eous 'na-t8n s en sno., me e

conjerser :e-d to he j must he conudered * >th respect :o as adahie Wah are e pheJ # :t mn N pmb.eN

cold We % pe ce f acJ+es 'or accurate Ae+R5:rg Ird the solume h e J s '.

g 9 or ma&ru'g N rem e > %

The se:und %;se., '

o

,4 g g,

,o he J N or-W 's. tg carku r ile j surf ace c o m f e'e.s san ' re a t 4

ss - e,es m m I re r?:f "

• e "e s f " d ' 1' TdI'T U

,, o,.eu y '

e.,

s, c.,.m^,,,

'" \\ f " 'U ^ I AO'E I OI

• IC E I e ' 's 6'

y f

N m-e m m c-oo, sre e s coc e r,.e.

cer - :esa..raer se-m :e ~ sure e

2cm m..m

.eam.e

,,e.ur

,-,I eas e cue '

t z

e,

Ur

• • >C

~ ! " re - e'ai s "i Red 7 e Pe-I"'I"C"'"

I "" "' " 2 e mes

. a

,,-2

=

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. e em- ' -s

-e-u.

s e r a I e

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{

y

, ps p

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a ()

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'f

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!a4 1rea e a re se" f e J "N

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v= -e : cJ xe: m 8uwe

~ n an he s eh af y 'ur:

a.

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• as he "dICJ d d "I

" " l' 'U d I $ J JE0' " O I \\ ' 'I U

1. L'

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\\n g

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dgjrirg ; y p 3 r.* p e.r jeg A

l ; _ a e, s ho a e sa., n u se eurose J 4.e r ce nu:h.

~a "e w re*e'"e2" gy

" e " N 'ef c ~ e n I.N)r fi r 2 'he Spec t -

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es are "eme teved ' researa inseu p arw e r:

• e c, os +e case a sm m a ~ er J lpj! spe; ; mens

'I s 'he raf.'1 <if'"e$

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IesI ht r ;Isfed t1in Iesfs A4 '

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{ g 4 m,

g pgskg g,q g y 3,37 gg + p g

l r heatre the es

'rea ~ e"s car ir"~

Nrs Aires or tubes h

De Nrrme d '"ese ' ream Fe C 4 '.ev e-S sM

pem h, q j ; p L.

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4 ' 'ha! 'he areas of

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}9 E SAI5dfJbC\\ f Ihf S IU C

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• Ces

'I' C r %i /e !()r s 4i e' k e " ' e s r n

• e s!'" g ()T s-e,

.,, g s_*,

u-

,ue.

' "a rm remmal of more exeru '*an n

p

,p er e u en.,e arru o ar s pe t - r, me, rev r

+'N

'M

' ' 'hff enars

• til ha s e htt'e = r tbe se on the teu JGPP'Pfd d'*f '"*f* M'f M f"' 'e

' e ~

• e c ' e,' ' f 1 b.

41'5 t Fises*r Isa!!s fli1* e s e r. In '

• e spec 'al J De tr % J r.

si rr s

", m a,

q ed

8. e s 4 t h o r tf a:!.* n a bim et:mes e"Lat ered "is he i npr mr

'e ' i pr.,

i. e i c ; arj'cs "a

c's g4-

., p i

a '

sw&m. :

a,- t ;,. -

Q w

s -

,e.

m9% ?

• %e

[ Elm g.

&O)s 5-

.m Q5 W

<d h

4

^ ---

' - - - - - - - - - ^

~ ~ ~

u:%

ges 4

?. e. p : yy y,_....

-W a w ~.

j

.g"N 7:te :*tfv Jr7

t t

3., :

J.~e f

.it. -

h A 262 for such specimens without waitmg until the end of 16.1.4. The corrosion rates are usualh re-denum-bear

~

the test period. A record should be made showmg ported as inches per month (Note 17), calcu-lar attack I which specimens were tested together.

Nott 14-If the multi-sample testmE apparatus lated in the following rate of corrouon equa-granular atti bec Note 10)is employed, a large number of speci-tion:

rnessure of t mens may be tesied in the large container provided Inches per monih = (287 x W)/( A x d = 1) other corros not proude.

19.3 After the specimens have been placed where:

IO""*

in the acid in the container pes cooling water i = time of exposure, h.

such as gen through the condenwr and bring the acid to a A = total surface area, em.

2 C0"*'

boil on the hot plate and then keep boiling W = weight loss, g. and throughout the test period (Note 15). After d = density (Note 18) of the sample g/cm' i

each test penod. rinse the specimens with Nort 17 -Cons ersion factors so oiber com.

anack anm water and treat by scrubbing with rubber or a monly used umts for corrouon raies are as follows:

nylon brush under running water to remove inches per month x 12 = mches per scar any adhering corrosion products, after which mches per month x 1000 = mils per ' month stainless sie thes should be dried and weighed. Drsing inches per month x 12 000 = mils per year 317L). It dc mah be facilitated if desired, by dipping'the inches per m nth x 8350 x densit) = milligrams tergranular i per square decimetre per da) specimens in acetone after they are scrubbed.

mehes per month x 34 M x densit) = grams per in these sam 212 The

~l Nott 15 -Care should be taken to present con-1.guare metre per hour i

in 8 = 6.45 cm-acid test mt j

tamination of the testing solution. especially by flu-orides, either before or durmg the test. Experience Nort 18-Values for the densities of stainless treaiment i

has shown that the presence of even small amounts steels to be used in the raic of corrosion equation ITIpes 316 of hsdrofluoric acia will mcrease the corrosion rate are given m the followmg table.

m tiie nitne acid test. It is not permissible, for also be use i

example, to conduct nitnc-hydrofluonc acid tests m

"'"I reduction in the same hood with nitric acid tests.

ceptibility to AISI 304. 304L. 309. 310. 3:1; ACI 79 316L and 19.4 For most consistent results, the test cr.s should consist of five boiling periods of 48 h A151316. 316L. 317. 317L. 347, 80 wrought pro each (Note 16) with a fresh test solution being 348 ACI CF;8M. CN 7M and weld me used in each period.

Aisiaan 73 1.3 Spec Nott 16-For specification purposes. those ex.

Alsi 410. 430 77 (Ty pes 316L perienced m the use of the test ma) by mutual

• The boihng nnnc acid test is somenmes uwd for esala-tizinc heat tr agreement, shorten the standard test to three 48-h ating the effectiseness of heat treatment for the chromium boilmg penods However, if with this shorter test steels hsied when so used. n acts as a um lated seruce u

ies for nnne acid seruce specificall3 rather than as an carbide prec procedure the rate of attack in the third period should esceed that in either the first or second indicaior of relatise susceptibihty to intergranular corro-heattnc used mon as in the case of the ausiennec stainless sieeis periods ta some pres sously agreed-upon estent, g

then the test should be contmued for a total of five 202 ReEort-Results should be reIorted monly used periods As an alternative, when the test is bemg used for inspection pnor to approval of steel for for the indisidual periods, as well as the aver-1250*F.

shipment, a procedure may be agreed upon by the age for the three or five test penods.

i purchaser and the manufacturer whereby the mate *

22. Summai nal will be released for shipment following satisfac-PRACTICE D-NITRIC HYDROFLUORIC

~~ 3 7 u

for) performance in three 48-h boiling penods with ACID TEST FOR DETECTING SUSCEPTI-fmal acceptance being dependent upon satisfactory BILITY TO INTERGRANULAR ATTACig The maten IN MOLli BDENUM BEARING STAINLESS tested in eac pc so, b ual agreement a cornbi at STEEI.S (63 ment: (1) of one 48-h penod and two 96-h penods (not neces.

sarily m that order) mstead of five 48-h test penods

! nealed)and may be acceptable for routme evaluanons.

21. SCOP' 1900 to 200 NOTE 19-See Pracuce A for mformanon on the Suenchedf

20. Calculation and Report most appropnaie of the severaliest methods asatla-20.1 Calculatiort-The effect of the acid on blej r the esaluation of specific grades of stainless the material shall be measured by determining test is tested the loss of weight of the specimen after each 21.1 This recommended practice describes treatment: (

test penod and for the total of the test pe-the procedure for conducting the 70*C 4-h.

a base-hne s riods. Such wetght-loss determinations should 10 "e rutnc-3 9 hydronuonc acid test as em-recened (cc i be made with the accuracy presenbed in ployed to measure the susceptibihty of molyb-If the as-rec 10

l s

u ~;

^

2092 neun *

?,.

s, :,y Y> y 5

o v

r x

u nm

~

"3

.Ar#

, -- -m.

m

~;

,Y T,4 3

- g,:

r i

A 2

l

\\

p

@ A 262 I

t

^'

~

}

l es are usuah re-

' Jenum bearing stamless steeis to intergranu.

step structure in the otahc acid etch test. a

-0 INote l't calcu-

'ar attack The presence or absence of mter-pornon of it must be laborators annealed to k

N d corrosion eg aa-granular anack in this test is not necessarily a gne a step structure and that sample used as u

i measure of the performance of the materialin the basebre spec; men isee foorrote c of TaNe

~ 'y.

Q 4 n t, a a

aiher corrosne e nironments The rest does 5 ).

not proude a basm for predicnr2 reustance to h7A[

'T'L orms at correw other than ntergranular

23. Rapid kreening Test 4g d

)

c h as ee,erai cerrouen put rg. or strese 23 i Before tesnng m the in 7 nerie

'c w'

l mros.or aaa y hs Jroquoric aaJ test, spec re s or +e stain.

V-21 I The li m h E <.-

mrrs 1 ~ hs dron e ric

ess steen as gnen in TaNe ?

n r

weene a f

203a 3 NcJ t e d dah the preapaawn of Jures gnen m Practse A. Otahc AuJ Etch

{e/

_ ',s-4 wJ 'es detem s 2 s e;'t h a mfergranular rap'J screermg test 'n accorjame aan prece.

I q

=

... r k e i+

res m 3

%s 1

h. r o m u m car N es m moi.Nesm nearmg Te st for C!asufication of Etch Structures of M'

! M% C stamiess steen i Ts pes 316. 11' 31^ L. and Starricss Steels Preparanon, etchirg and the f

= mis,v er H 'L ) It Jees not Jerect suscepnNhts to in.

classificanon of etch structures are described

~

mm = wm

.ergran Jar an.sa assoaan J e sigma phase therein The use of etch-struc*ure esalua'rons W

nun,m3 n te'e ume !s pes of staHew steel v.

n connection with the 10 'c nuric 17 hsdro-212 The lo 1 nurs _ 7 h s Jroduoric duoric acid test is specified in Table '

b

~

mJ test mas be used to esature the heat 231 1 Corrosion rest specimens having ac wr'es a ua+ew

're a t m e n t acordeJ a s. recen e J material ceptJNe etch structures in the Otahc AaJ crrown c a."

iTspes ilh and 31' stainless steel) It mas i p.

Erch Test will be largeh free of mtereranular b

\\

also be used to check the effectneness of attack m the 10 Fe nitric-3"c hsdroduoric aad

.f'

, Y. s 1

g " '.'

rehcnon.n catho content in presentmg sus.

test Such. comens are accepraNe *Hhout 1%

i

. 3

\\'

cernNhn to rapid mtergranular attack iTspes resurg m the 10 ~c nuric-3 C hsdroduoric g

g

.( g H et and 31'L3 It mas be arpheJ to ac J test All speamens hasing nonacceptaMe t

C

} p' %

4roueN prous i.nWJa c ohes t casungs.

etch uructures must be teueJ.n the lii 7 trd *e:J m etal aric-3 7 hsdroduoric aad test 4

~@J -

s

.1

\\;'e a m e ns.it estra hi* tarbon graJes g

- +

y

,,q M,-

i T pn 11

• L ard 3 i 'li are tes:ed af ter sense L Apparatus g,;

~:

m c e u 're r me % H ! 2' d > ro 12 5+ F F # ~50 24 1 The apparatus.s.Huur ceJ m F g

, [.

(($

M C'T>

• Neh n the rJnge or matimum 24 1 l TeJI Gimder! I hore 2f'l-The tests Q,

j y@ p[,

4 eare. %

,r carmde preep r 2ron The teneth of nme or are conducteJ m cs hnders of poht s msi chh>

p'

"$(

" 4P / " ' -

"e if m d used f or :5n sensdizmg treat men t

• dl ride ) (P\\ C) as shown in Fig in The test

?

Rereraih he ore or two hours The most com.

cshnders can be made from 12an (305 mmi I

"T I J be re pone '

wh used sensavire treatmerr n 1 h at lengths or l'+m Pk C pipe t ' +in 14 's S

• d ~* r

)

l ell as !F e ner 129 0 mm i *aH p hy enher of the tcHo* mg r*o tech-

[Qde l crmds r

l

22. Summars of \\fethod niques ill one end or each PTe teneth

,3 g

n piu eJ *rth a dai of ' m n P\\ C sheet and

.qd P E-K

[

.2 I h re t 'l0 Jrid ll' hdMM I bee / -

the Jnk n then heit *elded m ;'iate 4 thP\\C

[ j(-

he mrerial submdred for esa;ar on a i

gg g n gg g t

hiler rod. or l J ) ore end of eac h rice ieneth s

!s

n

. % "( 9

%I stNi t w

'ev d n each of r

• o corJJio"s or heat treat-plugged bv sah e n t -

• eldi n g a 1 cin N PS e

e I

9 eat i/) avreseneJ

1. comrren ab an-

p g);

(hheJule 401 societ-npe PW cap onto the i

T<.

l "ea ed) a"1 t J l !ahoraters-ar en ! 'or 15 at end at 'he pipe I

6 y-

[

N-g e.', g n e ;

o M # F l l' @' 'o l'Y L s. and

• yer 24 1 2 SfecWe" Hour'T tN ote 201-T"e

... v me-%

{t A

speamens mas he suspended < n the test solu-d' 3,' g

• d 22 IVef l l ^ l.

J"J I I 'l-ht"'e 5 5 non hs means of enher J speci'"en holder d as

$lf.,

te e her - The mate rial surmi:teJ 'or es aiva'ior w

Je%ribed an thn paragraphi or a TF E Ouor.*

'c u a c Je w ribo a 'estcJ r n cJ(h of !*o cim.! rions of NCJr cJr th m sI ri n g Ibfough dn J f'of flMe NoIC 3

I

..c a r me n t (!) a sers taeJ spesimen and 4 J,

JriheJ m one end of the speamen The spec

.-4 J- / e.

..'(

2h

'e i'

)(.

s h,G. ? ?

d 'e" e e t

' 'ase hne speame n w hic h usu alh s !

• e a s-men heade rs rras be m ue m c'ther of

• o Q,-

< c' re e sea umma ynem yye.,

,, 4. a$. -

.ns if,a i. n,23.m y :ewh at n E.

,n.o m-3 '"e b ret e n cJ gee me n a vs C u.)rocarh m t ubm g i l-in in s de Jia"'e t e r s a

{,d.

M,3, no r 3 hi> 4 a QQ K... wg. 3t -

i 4

o

• t ap -

I

' *c#M A dj "

j j;

t

@O[

V)KhWD.

M N.b b

N b

b

-^ '" ^

,,,a 2 g~ g y

. - w

.c..y. f* w..n...s

_p a..,

~

m i

R r.

h A 262 dnlled at one end to accommodate a %-in.

25.2 The intent is to iest a specimen repre.

portion of si to (4.76-mm) TFE-fluorocarbon rod. The hold-senting as nearly as possible the surface of the that sampic e ers are flattened into an elliptical shape which material as it will be used in service. Only such footnote c of h 26.2 Fill the is maintained by inserting the rod through the finishing should be performed as is required to ml of 10 G nur two holes and upsetting the ends of the rod remove foreign material and obtain a stan-tion and then he with a hammer, or (2) a %-in. NPS (Schedule dard, uniform finish as specified. For ver) l mater bath unti.

80) socket-type PVC cap is machined to re-heavy sections, specimens should be ma, duce the outer diameter of the cap to 1% in.

chined to represent the appropnate surface rneasured with a Nort M - 88

(27.0 mm). Holes % in. (6.35 mm)in diame-while maintaining reasonable specimen size-ter are then drilled in the bottom and sides of for consenience m testing. Ordinanly, red y,*g'o*'"',d

,n the machined PVC caps to allow free circula-moval of more malenal than necewar) will; ine corrouon rate

(

tion of the test solution. Smaller holes are have little innuence on the test results. How. '

,W when i

~

drilled at the top of the PVC cap to attach the eser, in the special case of surface carburiza-

, g $.C. lower TFE-fluorocarbon string. A loop of the same tion (sometimes encountered, for instance, in tion by means strmg is attached to each specimen holder and tubing or castings when lubncants or bmders string After a '

used to suspend it in the test cylinder, containing carbonaceous matenals are em-imens from the P oyed),it may be possible by heavy grindmg and acetone, dr l

Nort 20 - All poly (vinyl chlonde) maierials should be specified on the order as Schedule 80, or machining to remose the carburized layer,

ngid unplasiicized normalimpact PVC.

completely. Such treatment of test specimens d

fe 24.1.3 Consians Temperature Bar/t-The is not permissible.

26.4 Test or desired solution test temperature of 70*C is 25.3 When specimens are cut by shearing, der in additior obtained by placing the PVC cylinders within the sheared edges should be refinished b}

taneousis the a rack in a constant temperature water bath, machining or grinding prior to testing-each of the tw<

The temperature of the bath is maintained ai 25.4 All surfaces of the specimen, includ-for each maten 72 to 73 0 to offset the low thermal conduc.

ing edges, should be finished using No 80 or tivity of.he poly (vinyl chloride).

120 gni abrasive paper. If dry abrasise paper

27. Calculatiot 24.1.4 10 % Nitric 3 % Hydroffuortc Acid is used, polish slowly to avoid overheatmg.

37,3 c,feyf, Sand blasting should not be used.

Rares - The effe Test Solution:

24.1.4.1 Caution-The 10 % nitric 3 %

25.5 The specimen should be measured of the tuo spec hydrofluoric acid solution will cause severe and the total exposed area, including the inner measured bs de burns if it comes into contact with the skin.

surfaces of any holes. calculated in square the specimen.

Therefore, extreme care should be exercised centimetres-inches per mor in handling this solution. Rubber gloves 25.6 The specimen should then be de-h test exposure should be worn. Spilled acid should immedi-greased and dried using suitable nonchlori-men as follows ately be washed from the skin with an excess nated agents, such as soap and acetone, and of water and emergency first-aid treatment then weighed to the nearest 0.001 g.

where:

obtained.

26. Procedure r = time of e 24.1.4.2 A 10 % nitric 3 % hydrofluoric A = area, em acid solution (by weight)is prepared by mix-26.1 Types of Test Specimens:

%, = weight Ic ing 111 ml of 65 % nitric acid (sp gr 1.39),54 26.1.1 Types 316 and 317-Test two spee.

d = density.

ml of 48 % hydrofluoric acid (sp gr 1.16),and imens, one representing the as-received con.

l moly bde l

784 ml of distilled water in a polyethylene dition and one represeming the laborator).

27.2 Calcula annealed condition. (The laboratory-annealed carboy. Ftesh test solution should be made up 27.2.1 Type daily to avoid changes in concentration due to specimen must show a step structure in the The ratio of oxalic acid etch test.)

I es aporation.

'"'"

• d S PC' '

26.1.2 Types 316L and 317L-Test iwo the laboratory

25. Preparation of Test Specimens specimens, one representing the sensitized l

S'ned.

l 25.1 A specimen having a total surface condition and the other a base line specimen.

27 1 2 Type I

area of 5 to 20 cm2 is recommended. Speci-which is usually the as-received (commercially Sicel-The rati mens containing welds should be cut so that annealed) specimen. If the as-receised speci-sensittted spec no more than a %-in. (13-mm) width of base men does not show a step structure in the the as-recenec metalisincluded on either side of the weld.

oxalic acid etch test, laboratory anneal a 12

\\

u W__t'55* W y'35. M _.M. D uM M-M J

il,

~

. a 3 '. i 'q. ry g+A 2.-y

• 4 l 4 K :.,-f _.' '

'e f ~* ~ ~ f '"

i a, fr%5 ;.; - u: Tp

,. g y

t

,..,2

p....,.

Q.,

,,P u

.~y

'8' s,'A

~

m g,y

{ D ( $ ( I U L -..i ' ". J ' [ * ' g - Q Q i;.$

I dll ft

']

g I ': Y

.s l

,s-

ns,-.

v

^

.ne f

Jr.:. -

['

h

.[

l t

.a h A 262 r

ponion of it to gise step structure and use 27 3 Sigmficance of Corrosion Rate Ra-

.t a specimen repre-that sample as the base-line specimen (se:

rios-A value of 1.5 or less for the above 4

le the surface of the footnote e of Table SL

, seruce. Only such ratios indicates that the degree of intergranu-26.2 Fill the PVC test cylinders with 200 lar attack in the 10 ce nitric-3 "e hy drofluoric 1ed as is required to mi f10 ce nitric-3 c hydronuoric acid solu-acid test was not significant A ratio of greater and obtain a stan-

.pecified For sery

n and then heat in the constant temperature than 1.5 indicates that significant intergranu-water bath until the solution temperature. as far corrosion has occurred in the 10 C'c nitric-is should be ma-measured with a thermometer. is 70 : 0 5'C.

3 C'c hydro 0uoric acid test

,A l sppropriate surface

\\0M 21 -li 's important that the test solution Note 22 - Conversion factors to other com-i able specimen size i

t'e maintaincJ at 70 : o 5'C because small changes monts used units for corrosion rates are as fouows

! ig Ordinarily. re-

,n,ogon,,n,perature produce large changn in n

han necewury will the corrouon rate

' " C h ' 5 P' ' * " ' h " 12 * '"C h e' Pe r s c a r mches per month = 1t'00 = mils per month

! test results How i 26 3 W hen the solution temperature n 'O inches per month = 12 000 = mas per sear t surf ace carburiza-h' 'I 3 g $:C. lower the specimens into the solu-

'"C h P * "' h " 8 D "

• d'""

• m 'II's ' 3

• 5 i

ed for instance, in per square decimetre per Jag tion by means of the specimen holders or inches per month = 3a 9 = denuts = grams per f bricants or binders string After a 2 h esposure, remose the spec.

s uare metre per hour

~

J(

I materials are em-imens from the test, wash in distilled water 1

in * = 6 a5 cm2 p.

by heau grindin?

, ie carburized layer l and acetone. dry. and weigh Then espose the PR ACTICE E -COPPER COPPER SULF ATE.

b two specimens for an additional 2 h test pe-SLLFURIC ACID TEST FOR DETECTING d-t of test specimens riod in fresh test solutions at 70 : 0 5'C.

SUSCEirTIBILITY TO INTERGR ANUL AR g

ATTACK IN STAINLESS STEELS 47) @

.6 4 Test only one specimen in each cylin-L-

i re cut by shearing, der in addition it is preferable to test simul-

28. Scope I k j

be refinnhed by taneously the two specimens representing

).

381 This recommended practice desenbes i ' ' * $

each of the two conditions of heat treatment the procedure by which the copper-copper k,

specimen, includ.

ch matenal paluatd a

d using No 50 or sulfate sulfuric acid test is conducted to deter-Jry abrasne paper

27. Calculation and Report mine the susceptibility of austenitic stainless g"

steels to intergranular attack. The presence or

.soid os erheatmg 271 Calc:darton of Indardoal Corronon

~ used absence of intergranular corrosion in this test h.

g Rates - The ef fect of the acid solution on each

'JP. a.

uld be measured

's not necessarily a measure of the perform-

+-

of the two specimens of each material shall be

p. ;

ncluding the inner i

• ~

i meawred bv determining the loss of weight of

ulated in square i The test does not proude a basis for predict-i {.

- ~ ~ '

the specirren The average corrosion rate in ing resistance to other torms of corrouon.

uld then be Je.

such as general corrosion. pitting. or stress-

. [,,'

enches per month (Note __). based on the 4-y h test esposure. is calculated for each speci.

i w-l uttable nonchlore-

"E I N men as followt I and acetone. and 28 2 The coppe r-coppe r sulfate-sulfuric

?

I"' h I * "' h

• I q 7

• W I' I A *'"d)

O 001 g acid test indicates susceptibility to intergranu-i where' lar attack Jssociated with the precipitation of r:

g i = time of esposure. h.

chromium rich carbides !! does not detect

));

h 3

A = area, cm susceptibility associated with sigma phase

' ~

. mens l L Test two spec. lJ = weight low, g. and This test may be used to evaluate the heat W

as-recened con..

= Jensity. g;cm '. for chromium-nickel-treatment accorded as-recened material it y

yi.

I the laborators.

moly bdenum steels J = w 0 g;cm' may also be used to esaluate the effectnenew y

ora tory -a n n e ale d 27 2 Calculam"n of Corromm Rare Ranos or stabilizing element additions (Cb. Ti. etc i p

4 l

structure in the 27 2 I I5 Pes llo and 3/ 7 5tamlen Lecl-and reductions in carbon content to aiJ in i, F' Y

The ratio of the corrouon rate for the as-reusting intergranulJr Jt!JCk J/ 7L - Test two recened specimen to the corrouon rate for 28 3 All wrought products and welJ mate-

"J I h(f g the senutifed the laboratory-annealed specimen n deter-rial of austenitic stainlew steck can be esalu-q I

,e line specimen.

• 'n ed ated by thn test d (com me rcialk 2' 2 2 Tsres JinL and 317L Stamlen ll j' 2

K s-recen ed spec,.

Sterl-The ratio of the corrouon rate for the

29. Rapid Screening Tes 7

structure in the

""I'/Cd 'P'C' men to the corrouon rate for 29 1 Before testmg in the copper-copper

'T the as-recciscJ specimen is Jetermined sulf ate-sulf uric acid test specimens of certain Y

"ators anneal a M

- W,.Y ?

W.

.-..'[z $ $~

aw

ggp v

y

- ~

ype @fgG g

s 3

1p k 9 5,..;

g..

'm

(

i i

h A 262 34.3 All aussi grades of stainless steel (see Table 6) may be Nort 24-The solution will contam approu ccised" (mill an given a rapid screening test in accordance with g we

% of anhydrous CuSO. and It mai capable of meets the procedures given in Practice A (Sections 2 34.3.1 Specirt through 6). Preparation, etching, and the

33. Copper Addition stabilized grades classification of etch structures are described

.33.1 Electrolytic grade copper shot heat treatments therein. The use of etch structure evaluations or in connection with the copper-copper sulfate-grindings may be used. Shot is preferred for g

sulfuric acid test is specified in Table 6.

its case f handling before and after the test 29.1.1 Corrosion test specimens having ac-33.2 A sufficient quantity of copper shor '

i

[

ceptable etch structures in the oxalic acid etch

'E" d

"E.s is i be used to cover all surfaces should be taken t I

j test will be essentially free of intergranular specimen whether it is in a vented glass; attack in the copper-copper sulfate sulfuric cradle or embedded in a layer of copper shot' acid test. Such specimens are acceptable with-on the bottom of the test flask.

I Nou 2.L e

l performed to chee out testing in the copper-copper sulfate sul-33.3 The amount of copper used, assumin8,l and 0 03 9 m.ium f metak coppu is present, is not,

cartude precipiiam furic acid test. A!! specimens having nonac-an excess ceptable etch structures must be tested in the critical. The effective galvanic coupling be-l copper-copper sulfate-sulfuric acid test.

tween C Pper and the test specimen may have ;

importance (9).

t 351 The volu 30, Summary of Method 33.4 The copper shot or grindings may be i fate test solution 30.1 A suitable sample of an austenitic reused if they are cleaned in warm tap water l completely imme I

after each test.

stainless steel, embedded in copper shot or t

ude a mmimum grmdings,is exposed to boiling acidified cop-

34. Specimen Preparation per sulfate solution for 24 h. After exposure 35 1 r ar in the boiling solution, the specimen is bent.

34.1 The size of the sample submitted for tested in the same Intergranular cracking or crazing is evidence test and the area from which it is to be taken I all the specimen

• of susceptibility.

(end or middle of coil, midway surface and same 8rade, but it center, etc.) is generally specified in the.

The solution volu:

31. Apparatus agreement between the purchaser and the be maintained.

31.1 A 1-litre glass Erlenmeyer flask with seller. The testing apparatus dictates the final.

35.l The tes a ground 45/50 glass joint and four-bulb Al-size ant! shape of the test specimen. The speci-mersed}in amb lihn condenser with 45/50 ground glass joint men c nf gurati n should permit easy en,

brought to a bo (as in 9.1.1 and 9.1.2 and Fig. 8) are re-trance and rem val through the neck of the throughout the te

5' #

qie si e n rease is rec mmended for 34 a le 7 may be used as a guide to ng poi 31.2 Specimen Supports-An open glass determine acceptable specimen sizes. There ;

may be restrictions placed on specimen size b) cradle capable of supporting the specimens mue bump ng of the and copper shot or grindings in the flask is the testing apparatus.

used to support spe.

rec mmended.

34.1.2 Specimens obtamed by shearing per shoi to io 1( pn Note 23-It may be necessary to embed large should have the sheared edges machined or

' ' U ' "" " " ' D

specimens, such as from heavy bar stock,in copper ground off prior to testing. Care should be,

35.1.3 The tes shot on the bottom of the lest flask. A copper taken when grinding to avoid oserheating or i boiling period L cradle may also be used.

" burning." A " squared" edge is desirable.

Fresh test solutior 31.3 Hear Source-Any gas or electricalls 34.2 Any scale on the specimens should be !

test were to run heated hot plate ma) be utilized for heating' removed rnechanically unless a particular sur-l adherent copper i the rest solution and keepmg it boihng face finish is to be evaluated. Chemical re-l may be remosed t m val of scale is permissible when this is the throughout the test period.

centrated nitric ac case. Mechanical removal of scale should be

32. Acidified Copper Sulfate Test Solution accomplished with 120-grit iron-free alumi-

36. Bend Test 32.1 Dissolve 100 g of copper sulfate num oxide abrasive.

361 The test (CuSOc5H O) in 700 ml of distilled water, 34.2.1 Each specimen should be degreased through 180 deg a add 100 mi of sulfuric acid (H;SO., cp. sp gr using a cleaning solvent such as acetone, alco-the thickness of th 1.84), and dilute to 1000 ml with distilled hol, ether, or a vapor degreaser prior to being water.

Iested.

14 3ng? :er i

e

---

w-,-----._-y-,,.-

-p y,-___-.c-,-_.,..,,9.,a-

.-,--.yvw-,.,m,_

-._____s-----s.-,m-y----w-_

m m-

i a

N'~

W

^

e - -

n gy.qy :.=:

m 4.:.5

. k "Tg_

1 1

h A 262 F

y 34 3 All austenitic material in the "as-re.

Fig 11) In no case shall the specimen be bent

'4 sotunon wdt contain a ppro u-ceived" (mill-annealed) condinon should be oser a smaller radius or through a greater e

i, of anhsdrous CuSO. and le capable of meeting this test angle than that specified in the product speci-4 34 31 Specirnens of estra low carbon and fic: tion In cases of material haung low Juc-

}

haion stabilized grades are testeJ after sensitizing tility, such as seserely cold worked matertal. a g

heat treatments at 1200 to 1:50*F (650 to Iso-Jeg bend may prose impractical De t e r-f w

tic grade copper shot or 5 5'CL which is the range of maumum car-mine the maximum ang!e of benJ without h

,.{

used Shot is preferred for T he m'ost commonly used causing cracks in such material by bend:rg an 8

' l '4 h de recipitation i

ng before and after the rest sersm ing treatment is I h at 1:5WF Care unrested specimen of the same configuranon

! ent quannty of copper she uld be'ta k en to as oid carburizin e er nit rid-as the specimen to be tested y

sh be useJ to coser all surface.

.n the specimens The heat treat [ng n best 3h 11 Duplicate specimens shall be ob-7 4hether it is in a sented glan

[rncJ out in air or neutrJI salt lained from sheet material so that both sides f

ed in a layer of copper shor the test as

~

ep i,s of the rolled samples may be bent through a 1

rtormed to check the effectneness of stabihzed 180-deg bend This will assure Jetection of M

une of copper used. assummg W o 03 % maumum carton matenais in remong intergranular attack resulting from carburiza-dlic copper is present, is not carbide precipitanon. hence. intergranular atracs j

g crive geh anic coupling be-the final stages of rolling y

35-W Condihn, 1 the test specimen may hase ME U - Ide nn h the duphc3te specimen in M 1 The solume of acidified copper sul-such a manner as to ensure boih surfaces of the ser shot or grmdings may be fate test solution used should be suf ficient to sheet material being rested are subjected to the p

I

cicaned in warm tap water completely immerse the specimens and pro-tenuon side of the 180-deg bends i

b 3 (8 ml.cm;) of 3612 Samples machined from round sec-a side a minimum of 50 ml,in specimen surface area tions or cast material shall hase the cursed or

.h cParation 3511 As mans as three specirr ens can be original surface on the outside of the bend r.

of the sample submitted for

'ested in the same container [t is ideal to hase 3613 The specimens are generally bent

~

from which it is to be taken MI the specimens in one Bask to be of the by holding in a sise and starting the bend with g

if coil. midwas surface and same grade, but it n not absolutch necewar) a hammer it is generally completed by brmg-

)

generaih specified in the The solution solume-to-sampie area rano n to are the two ends together in the s ne Heasy

~

9

~

5

en the purchaser and the 5e maintained specimens may require bending in a inture of

(~

~J

apparatus dittates the finai 35 1

The rest spec:ments) shoulJ be im-suitable desien An air or hsdraulic press mas L

ihe test specimen The spect-merseJ in ar-bient rest solution which is then also be used for bending the specimens should permit easy en "ro u gh t to a boil and maintained boilin?

3h 14 Tubular prod'ucts shoulJ be Gat-k in sal through the neck of the throughout the test period Begm nming the tened in accerJance with the Gattening test.

'est period when the solution reache3 the bor:-

p:escribed in ASTN1 \\tethods and Definitions I

' mas be used as a guide to ing point 4 3 0 for \\1echanical Testmg of Steel ProJ-able specimen sizes There b

4-Norr 3 steasures should be taken to mini-ucts.

y a placeJ on specimen size bs

,y, g g,a s me solunon. hen giass craates are alus meJ ro suppJrt speumens A small amount of cop-

37. Evaluation c=

g ens obtaincJ by shearing T shot i' to It' Petesi on the bottom of the flau

" "" C 'h '# " ' * P"'P"

r gg i7 shcared edges machined or under lo* 15 to 20 = ) magnificanon (see Fig

{

io testing Care should be 3513 The test shall consnt of one 24 h

12) The appearance of fissures or stacas indi-

.~

mg to avoid uscrheating of gj.ng pe riod unlew ot h e r w ne specific d cates the presence of meergranulJr Jttack (see I

bl uared ' eJee n desirable Fresh tesi solunon woulJ not be neeJed if the Fig 13) on the specimens should be eu aere to run 4% or esen 72 h (if ans 3711 W hen an esaluation n quesnonable

' fj Ty salh unless a particular sur-Jdherent copper remams on the specimen. it (see Fig 14), presence or absence of inter-

't ij-le esJluJtcJ Chemical re-mas he remosed bs a briet immeruon in con-granul[r attack shall be determmed bs metal-

I permnuble when ihn is the centrateJ nitris wJ at room temperature i lographic esammation of a longituJinal sec-d 4

3 remos al of scale should be tion of the specimen at a magmnsanon of liill

'i b 1 1 iL grii iron free alumi-

36. Rend T est to.' N s

[

C 36 1 The rest s pe cim e n shall be bert h ent sus h as ateione. alco-15e thn;k"cu of the speumen being bcnt nee va lii

^

hb cumen should be JegreascJ through Isit dee and oser a diameter equal to

, m]h.,a

[

1. 4 s Mr $mrai Pni. 3aL 5

.C i

or deceaser enor to beme 4

t a

U i5

,e

e. ? s '

n&

A

-Q6.b k

~,'. S.. = 1 !

C kWTIS~7 f

ff f

Q

[

,-v----

~

l M ' '" ~

4.t.*.

t, y d 4 +'

'is

@e A 262 NOTS 28-Crackmg that origmates at the edge Noit 29-Cracks suspected as anung through pitLE 1 A ppi,rehe of the specimen should be dnreparded. The appear-poor ductihty ma) be intesogated b) bcndms a ance or deformahon hnes, unnLles, or " orange sim:lar specimen which was not esposed to the boil.

g %,,,,

peel" on the surface. mithout sccompanymg eracks mg test solunon. A usual comparnon between

,,g,,,,,,,,,

or fissures, should be daregarded also these specimer.s should asust m mterpretation.

,,,g p g a,nn :-The n=4ti REFERENCES j

(1) For ongmal descriptions of the use of etch Reagents. Specifications Recommended by structure classifications, see Streicher, M. A.,

Committee on Analytical Reagents,' Am Chem. Soc., March 1941.

" Screening Stamiess Steels from the 24Gh (61 For onginal dewnpnon of to '"< nienc-3 e',

sise ma mat Nitnc Acid Test by Electrolytic Etchmg m ACP Ct 3 Cl Omahc Acid," ASTAf Bullerm, No. IMB, Feb-hydrofluonc acid test, see Warren. D, "Ni-ruary 1953, p. 35; also "Results of Coopera-inc Hydrofluonc Acid Esaluation Tesi for tive Testing Program for the Evaluanon of the Type 3!fiL Stamless Steel," AST4f Bullerm.

~

j Omahc Acid Etch Test," ASTM Bullerm, No.

No 230, Ma) 1958 pp 45-5A 195, January 1954, p. 63 (7) The use of copper to accelerate the mtergran.

wnc Ac,d Tes ::

(2) For ongmal dewnpuon of ferric sulfate-sul-ular cortouon of senutired ausieniac stainless boa,cp wuno, func acid test, see Sireicher, M. A., " Inter-steels m copper sulfate sulfunc acid was first

~

devribed bs H. J. Rocha in the discussion of a tamiess Steels: A Ferne Sulfate Sulfunc paper by Brauns, E., and Pier, G., Stahl und C***'**d'N' ','

kranular Corrouon Reustance of Austemtic tcy

,,,,,d Acid Test," ASTM Bullerm, No. 229, Apnl Euen, Vol 75,1955,p.579.

p, 1958, (STP 95), pp. 77-86.

(8) For origmal evaluauon of the copper-copper

,y g,,

(3) For ongmal desenpuons of the boihng rutnc sulfate sulfunc acid test, see Scharfstein, L.

3g, 3m R., and Eisenbrown, C. M. "An Esaluation 3g d FM CF.t I

acid test. see Hue), W. R., " Corrosion Test of Accelerated Strauss Testmg," ASTM STP Ead4 rain in su pa-for Research and Ins ction of Alloys,"

Transacnons, Am. Soc. bel Treatmg, Vol 18, 369,1963, pp. 235-239.

1930, p 1126; also, " Report of Subcommit-(9) Subtle effects due to vanations m copper sur.

-,3,3,,g,,n,,,

face areas, galsanic contact, condenser de-

,,c gm c, tee IV on Methods of Corrosion Testmg, Proceedmgs, Am Soc. Testmg Mats., Vol 33, sign, etc., are described by Herbsleb, G., and

,w,,,,,,,,,

Part 1,1933. p.187.

Schwenk, W., "Untersuchungen zur Emstel-(4) For details, see DeLong, W. B., "Testmg lung des Redompotentials der Strausschen Lo - '

, u,,,,,g

, To dais' eo dat sung mit Zusatz von Mettahschem Kupfer,'

Multiple Specimens of Stamiess Steels m a Corrosion Science, Vol 7,1967, pp. 501-511.

Modified Boihng Nitnc Acid Test Appara-(10) Brown, M. H.," Behavior of Austenioc Stam-rus,* Sympossum on Evaluarson Tests for Stamless Sicels ASTAf STP 93, Am. Soc.

less Steels in Evaluanon Tests for the Detec-Testmg Mats.,1950, p. 211.

tion of Suscepubiht) to Intergranular Corro.

(5) See Indusinaland Engmeermg Chemistry, Vol sion " Corrosion, Vol 30, January 1974, pp.

17,1925, p 756; also, "A.C.S. Analyucal 1-12.

Pracuce 8-Ferne i

Pracuse C %inc I

Pracuce D %ine Pracuct E--Cope TABLE 3 Use

• ,o t s -G r ade-noi ombie en the e Grade 1

l AISI 304 AtSI 30aL AISI 3tti Alst 3tt>L A:51 317 AISI 31'l AtSI 301 ACI CF 3 ACI CF-8 ACI CF-3 ACICF4

• Spromeas h r

16 O(

M h M N %,"MM6MN,k3

~

- wJ

. O,-

3

~c:imm a ___f eW w--. _.,,i, m s.

(

l WM*'*0rsM.

s3 o

L-s h A 262 1

$ fected as arismit through TABLE I Apphescos of Evaluartoe Teus for Deteenns Senupnbdity to lesergrenaler Arisch a 4asleeirw stainless

'g invesogated bs bending a

seeet, p

E N

.as not e s poscJ to t he boil-sm I-For w arros.e een W w of wep.lu, m iniererMr am mW are & aw a m

'b=

sual comparaon between grad s of usin. css weeis.n h.sh thes ma. %e fou d Thew tsis ma, caatain stades of weels n add oon to show g ca ia n

suist in interpretanon es b s

a d corevs.on teu is applicable but act t*e onahc acid eich teu son :-The oubs md etch leu ma, be apphed to the grades of uamess siccis trued in the rectaneies

• hen u sed a y

conneu ton m a h the teu ndiseed $s the arrow g

01t AllC ACI E TCH TEST r

N I

b

, nons Recorr menJeJ %

l

[

{

g.

~ g ~,

l h nc al Rencan.

A rn fAISI M4 LG4 L 116 1941

1. M liAL ll? Il?L Afsl 116 Il6L ion of 10 "c mir's 1 7 sl5l= M4. iga t b

(F 1 CF 4 ll' )l'l f Kl I

t see W arrea D u l' CF1 CF<

I M.

f

,d Es aurmn Test tar l

C F I M C F il M k.

L Steel ' A S T if 8,de: n h

pp 45-5$

Copper Cspeer Sulfate E

F em suh Swifanc Acd acce!erve the mterittan-y, nc y, 7,y, 7,3,,,

y, g,p gn d Tesi a 4m 3

Teu s i 0 m.n Soihng Teu i 4 % u 'O C i N# * * 's wiu istzed Justeninc wa.nien i,c, n,,, %,,,

'**"'3"'

'n bodie ocai te-wifuric Jud was first d

i (ha in the Jiscuwon of a O'""*"'d' N'

O ' '" '"" 'd e

,n 304 C h romiu m ca r bide in 316 Chromium care de in 104 and,P e r. G. Lahl and 304 L CF ) CF 4 104 L

}l6 Il6L It'

)l6L 31? 11'l 104 L 316 Ilot.

11' p 59 m wra w ar de and II'l CF ) CF4 It'L 321.34' in of the copper capper

' ' ' ' ' pe a se

.a*

lie C % rommm care.de aad s.sma est, see hharfuem. L

"*' "' " 32

' " ' ' ' ' "

• C"*

C N1.

An Esalu4non 147 C F 3 M C F 'I M 9M' s Tesong. 4STifSTP 39 E nd s'a a n el s'ades 4rtanoen in carper sur.

• AISI * *'"" I' " 'ad Y ee' law ouie des.g aanoas for austemoc u aress ure4 contact conde mer Je.

h.

• • C3

^"*'C""8I"""#'d**'"""'

ed by Her5ie5 G ana

"' " " " " d ' '" " ' " # " ' P r "'d ' " ' 5 ' 30* 3 ' O

'"d ' ' S ' ' ' O # 30 ^ ' na AC I C N. ' u r1uchungen zur Ernstel-

• """*"'d'"'"""'"***"d'"""""'""'"d eats Jer siraum$en Lo-b b

Me!f a!-% he ') Ngprer l7,196' pp 0:1 511 l

uur of \\uuem c Srw on Tesa f ar me [ eiec Tm E' 2 4 @ W of 6 h Teu

'o Inter c aNar L}orro-i M. la"uv 6 i 4'4. pp Ai3t c,4ee sa

___ 4C: craae so j

s.

Pmt.te 8-F e r c %. fee %ifurs Acd Teu 104 M4L De li6L 31'

~CFT C F 4 C F-)M

)l?L C F *M E

P wne C Nanc Aud Teu 304 Mel CF 4 CF 3 I

i P ause D-Nar< Hidwh r c Aud Ten l'6 Ji6L II' il?L f

Practice E-Copper CopMr Swifate Sulfunc Acid Teu 104 104L.}l6 Il6L. }l' g

n't m 347 y

i E L 4

T4ati 3 tse er n ich struciere c1. fw.eion. fr he os 4.e 4cid F teh Test asth Ferrw selfele-selferw Acid Teu son -c,ae, usi m a d 34' canno. se wreceed 'setwe 4ese s,adei m. conica a i,x or,,m a pha,e.n<a,s n

9 f. 4 hic 3 ' *e ei69 struw u te ui *Mah*at sauw f a cid s'Of'J % ion a t "f 'f rt iu'Ialf S u'Iur 't' acJ'cu orae mepo,le w si,uu-e, s ~ rpmae ~ sm

-e,-

m stSi Ma Sie p Duei E nd Gere I i ll Do s l

Y[

usi w s.ee D a Ead cr&a i sn Da s I

sisi 14 Yep Duai E ad cron i i 11 D.i d i

[g

,,( j l

i st%Istel

%ep Dual Ead Gera 11 ll D'i d sisi it' vep Dual E ad Grea i l 14 Ddd

A I & 11 Doch l F sisi )i'l vec Dus E ad Ger a y

Aisi m some T

ACI CF 3 Yep Da Iwurd Fernie P*n D1 h l a'e Ne a d t -

D%aes

. x' p

6 s

SCI ( F 9 Siep Dwai Iwlated Feroie Pws De laiemeadr% Dmacs t

ACI C F-lM Yep Duo Iwurd F ernie Pws D%h laie oeadra s D ic rs I

a SCI C F eM Ster Duai Iwlated F ernte Pain Dit c h l a r c +ccad r*is D4sies J

4 i

E*%

uemuu 5e tenied 'a t ac

• e*' s suifee voar i.

6 d te's

• s reme a. 'sa.ms cw sira a

r e

m,$

x 1,b.h., *.6 are.

a.

. gI g e d. +

k

++

1

h A 262 TABLE d Use of Esch $sreetere Claeseflessions from Osalie Ac64 Eeen Tess Mth N61rit Acid Ted Non - AlSI 316. 316L. 317,367L. 347. and 3:1 cannot he screened hewww thew ucch mas waiain isma chaic noi visible in the etch uructure This mas cause rapid interpranular aiiach in the narw ased test Nonescepiahn lish Siructures*

Grade Acceptable lich Structures s

AISI 304 Step. Dual. End Grain 1 Duch. End Grain 11 Alst 304L Sier. Dual. End Grain i Dnch. End Grain il Duch, laserdc drnw Onches a

AClCF.h Step. Dual. Isolated Fernte Poots ACI CF 3 Sier. Dual 1=ol.ned Ferrue Pooh Deich. Interdendenic Dushcs

• Specimens having the+c structures muu he tened in the nnric acid test

,y m%

fa Use of Elch Sareciere Clasifkseiens from the Osel6e Acid Elth Tess Meh 10 4 Nterte 3 % H drofluorie Ae64 3

TABLE $

Tess N * * '" 'P' '"["

"d"'**'I"

Asseriable Eich Sirustures Sirvi;iures Grade T reat ment AlSa 3 6 A prece,*cd*

Step. Dual. End Grain I and 11 Dach AISI 317 A preces.ed

• Step. Dual. End Grain I and 11 Onch As reces.ed Siep. End Grain i and il Dual. Dach AISI 316L Senuaired Siep. Dual End Grsin I and 11 Dach As-received Step. End Crain I and il Dual. Dach

"'S'3

Senuiered Step. Dual. End Grain I and 11 Dnch

• Specimens having these structures must be tested in 10 % nitric.3 % hydrofluonc acid test.

'If the as. received specimen shoes a dHch siructure and the HNOrHF test is to be applied. then a duplicaie specimen must be laboratory. annealed in order to produca a baw hne specimen having a saep uructure The laborators.annea ed ~

s specimen f uep structure) along with the original as. received specimen IdHch siructurelis subjected 10 the HNOr H F iest The final cenence is then the reno of the' corroseon rate for the as received specimen to the corrosion raie for the labora.

tory.annesled specirnen' % hen the omalic acid etch iest is used eith the H NO..HF test for Types 316L and 3t?L. the as. received specimen sh lf show a step structure (free from precipitated carbidest if si does not, a port on of the as-recened specimen musi be laboratory Thes reewre.

annealed to produce a base.itne specimen having a step structure and that sample used for the HNorHF tes ment is necessary because the base-line specimen must be completely free of intergranular attack in the HNOrHF test in order to obtain an indicative raue of the corrosion rate of the senutized specimen to the corrosion rate of the basc4pe specimen.

TA8LE 6 Use of Each Structure Class fkstions from the Osahe Acid Etch Tess with the Copper Coppee Selfsee-Sulfeeic Acid Tess Non.

2*-

Grade Acceptable Etch acceptable Each Structures Struc-tures*

Alst 304 Siep. Dual. End Ditch Grain I and il AISI 304L Step. Dual End Dach Grain I and 11 AISI 316 Step. Dual. End Onch Grain I and 11 AISI 316L Step. Dual. End Ditch i

Grain I and 11 8

AISI 317 Siep. Dual. End Dach i

Grain I and 11 AISI 317L Step. Dual. End DHch l

Grain I and 18 Alst 321 Siep. Dual. End Dnch Grain I and 11 AISI 347 Step. Dual. End Dnch Grain I and 11

• Specimens hasing these uructures muu he tened in the corper-correr sulfate sulfuric acid test p

i8

.NW 4

%Qf2ki G

as W

g 6)

H 4

Q

i N

3 A

g 4[h A 262 W

i n..

TABLE 7 Sues.f Tese Specimens Tous own %.sric Acid Tess

'e D T,pe or wi,,ul Sue of Tesi Specimen

ueets mas sonuin s,ema chase not 4

4 gay

.f 7

• ros,ekt sure or r d o

• onacceceante E nh Strwiu es' L p to, in in diameter inct FoH diameter bv ) in tmin i z

r M",

ty d

Over

'4 in in diameter Cylandrical segment '.m i

Desch End Guin 11 Duch E nd (.rva 11 r hic s e= I.n i m a s,..de c?,j D.lch inredend t m D t s

-1 g>j.

e.

Dit c h lescede dr ts D.taes bv ) to ?.n ions

• n 4.-

ss N

a ros,ekt t hre r sterp piarer

?

TY

>r *!ar tot 92 produrrr Lpm

..a m cm mci

Fu l 'hica nen bv e to I in

}

e

..de B. ),n i min i ion e g

O.er. in rMu t

6. to 7 in thsc h 9, e to I to %.%eme-3 % H.,drott.oric Acid 4n.i

) in s min,

m...

de ev t

I Nomau couede f.x" 5

Ts, bin g g

v r uc t u re s*

Up to l ' s m m diameter.

Full rice t.a..de

,gy f

Over l' : in m daame'er A circumferential se,meni )

{

.n i m.n, o., c., <r om.

y DM De 3 -'"

• 48 h6*

U" os --

• W hea deadine sah soeurnens, the curved surface shall l

m, ~

~,,<e ne he,d c

one.na.e sn.u he a orie,n. 5.aace or ine maierui g,,y nder test and it sha*l he on +e outside af the bead Couf e

4 coned Me* 2 dwphute ipcomen

?'

ar crore the 4 >umrs vio,, ca "d

2::::"::: :he"':c::

NW

_,,,,,,,,,,g,,,,,,

m,,,,

},s q 3, -.-re~

re ~ ~~~-.~

l.<~...e..e_.,.n_

s -, D--, - ~ n -

j. ei.ed s pe-c e,... e, a n,,,,wr,

• d '* ' d h e ' * " " * * * * 'd o a ' ' ' "' ' 6'

• d a

'r the H NO, H F 'cu T ha reg., ce 3r 31tJt b

.M 'me H Ns), H F.gy n

he corrown are

>( en e wage, ce

1. Iq i

g

-n 4.

c: %,

'Q

/

't 5

5

.o k,L j 'hEh.(.,. 'l h; 'c$

,. ry.

. s.,.

s.

j.

.w

.c.

..'Y

, \\> 4 c

~

t

.k

'x e

d

'G,b 6a

,s

-G.,;

j

-5:

e^

gd

'~

t s.

(

" @g T.

c.

.L 3

I.S ' 'nT, 3

,-r

.e -

i

,, a.

i, L.

m.g-a v

w.

s s

7 %

t,,? J s.,

i 6, 6,

),

w..

x n ;.e v

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