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

,t l g

v. l &

l

• W - _

b

?  ;

W %.u, w cs,m Il stance #: ANSI / ASTM A 262 - 77a -

es . *-

a

=

% .W. t L

'[ E ts Standard Recommended Practices for Y8

! DETECTING SUSCEPTIBILITY TO INTERGRANULAR A ATTACK IN STAINLESS STEELS' s s e m. s %c; me, a c e .ca zes e,o i r 4.-

. car M < ' g

• 4' al p e et e

im %c gase of ec.:s c ect me a ,.e , ..,me 1.

i w e.rr% ai et the ,cae '

' age re.nica  :, w .. . r

-ame,+,

,,, ,w - Aco-N: n pa ce he gg g f j ( 3' e g

• we .ggr c e a

,-a, a r .ws ,, % , e,,, ,r r 4, a .c , o , -

mses <

• s;rt . s a..o , a waa.c e , o ,, o , 4, n,,,, ,. ,,, , e o,,,m - a & ,. g w ,, . ,, 4, l 1. Scope -

[13 The osabe acidn etch test bs a r a pid

&c11 Thesefue foHew:rg recom rests mended practrees cover ' rnethod of idemnync. simple e:ch:re. l "

i : 1 Fwnce those specimem of certain uamieu steef I 4 - Osahc Acid E1ch Teul ,

tr ClawfNanon of Etch Structures of Stain.i grades whah are essennalk free of suscepn- N tess 5teek r %ect:ons 2 to 6. mclh Nb to intergrandar anan awoaated *nn E chromium carNde prearnates These spect-i 1: Fwru e B - Fernc t Ud Teu for derecnne wssernNhts to mrer. C """"" Sulfate sulfuncj CoMNn Tem rates w i,th.ena:n hJs e lo*

"' d n d *' f' k f' Cd" DC Ch*"

creu!ar

>o i s mcm anack m stamleu veek (see $cenors i

nated Iscreened) hom teump as._ 3ce r_'a; _ _

( Ps.n e c - surn Aod Teu for de. 14 The fernt wuate%nu is aad teu the

.rc vcernNhn m ir ergrarwr anad m W.r!cu u

"""C d"d 'e " dro 'he "C ~ h ' d roo' -

I rek a!% t see Nee mn 14 to :l' mdi aad reu are 5ased on *ep b 2erma-ie D - N a ric-H s droiluoric no s and. thus pros tde a Quar utatn e mea. i ,

,k Nar J Teu Wr Je'echre anack su cernNh's lo in'erwre o s

e relanse pe@rmme of speccens m wh hdenum.beanne aus- esalaa ed in cemrau. the copper-correr sul-nx cam:ess ueek nee secnons, :1 io :-

l Id

• H d "' 3 o d ' e" " Da s' d "" "sual enamo

,' d and -

!15 nanon of bend .

Pra ru e E - Copper Copper Sulfate- Teamens ard. rherefore daw -

Uanc Acid Tes: for derecong suscernNhn u res the speamem onh as accerraNe or non-  ;

.st- d "'I'd N' ._

'p [ kmonjs,tercranular attack m udmlew ueek (see I'" " * " '

!  % ' i: O'pper sulfate wlfunc aad teu et the . D h The foHowmc f actors cosern the apph- I' f"C ""# ' '"U ""C 3 d"  ;

hr of these rewmmended prachces '" % I' d * h

': 1 'ne esahc aad etch teu *in prouce the re- .)

SuscernNhn to intercranular anni ped mimanor 1r the shonest r re AM 8'"

c;df ed *1f h the preClpliai P of chromidm edes is readih de'ec'ed ir au f n e tem Id # d' ""## *

' 5 2 2 Stima phase in

• r.iuc it ch ro miu m- c'#C" * # #

E

'ebmoh bdenum ceek whwh me or mas weamem m

Nenebewp Nah w e usiNe m :he mwrocrature can resua *' ' ' d "Pl' 'IN 'I4-

- 'Nn 'l' 1

cerrosion rates on k m r.ine aad 3"d 3I1' -

• 2 i Nema phase m 1:tarwm 1

I hs or solam-g' N'" caNhled aHos s g 'NNe m the microcruture w hhh me or me no:

ne,e rew- e ec a prw (es a.e

""" # " S I "

and Re s ed Adom C"" " A'l *\" orac me s,rma4 5 ' ' ' '" Y " '

l

~ . tan resuh in  %,No- me, Ae1la a*J are m e d ce resW m M r ,',m, c sSh corrouon rates m Nuh the

- n'incC acid m","e' '" 'o<

.nd 2 ""' 'PP c,-

ve+ e <. c e n e Teu q I

t ulfate-sunanc wd .uunons e.~n r"n' 2# ,

oruun SM , ' -a 2

• w, ',e:

~" " ., ^A : ~

e e m,r. = r

, i i

!' 8505010128 841011 PDR 1 G ADOCK 05000413 s

PDR -

i 7 4 .

'% 1 V .

.c t 1

l

s" $$0E5? Cy l 5"$5

< f,

{E

.n p

=

I b 00LKETEE t USNRC

.N

-c fl1 4m

'E '85 APR 25 A10:58 s

( L Li 25m I t $g e s y "W 5 6Ss E ~

OFFICE Or SECRtTART 7

! GGE gS S 00CKETING & SERVICI N

O l  !

• k7 e=

E a

BRANCH et t 1

BP y i

' e W

j i 4 6' e

t

. W tr b ,

1 k h A 262  !

senting as nearly as pomble the h ;'

w hich represent steelintended for use in mtric acid environments.

2.3 The grades of stainlew slech and the matenal a'it *'ll be used m scru j hot acid tests for which the omahc acid cich surface finishing should be pei l.6 For AISI Grades 316.316L.317 and test is applicable are listed in Table 2.

6 317L only, the nitric-hydrofluoric acid test ,cquired to remove foreign mai i W may be used to provide test results in 4 h.

2.4 Extra low carbon grades,such as 304L. ' tain a standard, uniform finish a

? 316L. and 317L. are tested after sensiiizing 4 3. For very heavy scciion 1.7 The 24tkh nitric acid test must be ap-1 se heat treatments at 1200 to 1250*F (650 to should be machined to represc

• . 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 F*

subject to end gram corrosion in meric acid are submitted to the oxalic acid eich test. The will hase little influence on the 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.

listed in Table I for which data on the applica- bunzation (sometimes encount ,

3. Apparatus stance m tubmg or castmgs *t tion of the oxalic acid each test and on their or binders containmg carbonace y- performance in various quantitative esalua.

are employedi it may be pow tion tests are asailable. 3.1 Source of Direct Current - Batter).

[ generator, or rectifier capable of supplying 1.9 Extensise test results on sarious types about 15 V and 20 A. gnnding or machinmg to compi the carbunzed surface. Such tre.

of stainless steels esaluated by these practices 3.2 Ammercr- Range O to 30 A (Note 1).

have been published m Ref (10).2 specimens is not permnsible, e ,

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 less steel or preferably, a 1-qt (0.946-litre)

A SIF AT NO ETCt Tt C. 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 men to be etched.

3.6 Aferallurgical Aficroscope- For exami-plate, weid heat-affected zon ,

{

p acceptance of matenal but not for rejection of matenal. This may be used in connection with nation of etched microstructures at 2501o 500 metal. Scale should be remos ed to be etched by gnnding to an i diameters. fimsh on a gnnding belt or u other evaluation tests to provide a rapid

,_ 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

%. and %. or finer. This poksh i miergranular attack in these other tests. Such a stainless steel beaker or a piece of stainless 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 ;

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

, ious hot acid tests. requinng from 4 to 240 h i

(- of exposure. These specimens are identified 3.8 Electro /vic-Oxalic acid. (H:C.Oc .W heneser practical. a polished e by means of their etch structures which are 2H:0). reagent grade.10 weight G solution. or more is desirable if any ci I classified accordmg to the followmg cntena: dimension is less than I cm.

1 Non 1-The vanable resistance and the amme- length of I cm should be polish.

j 2.2 The oxalic acid eich test mas be used to ter are placed in the circuit to measure and control screen specimens intended for testmg in Prac- 'h*'""'"' "'h' 'P"'**"'* D*h'd' asailable length is less than I cr section should be used.

tice B- Ferric Sulfaie-Sulfuric Acid Test. .

4.4 Eiching Solution- The -

h Practice C-Niinc Acid Test. Practice D- 4. Preparation of Test Specimens 4 Niine-Hydrofluoric Acid Test, and Practice for etching is prepared by add C 4.1 Curring-Sawing is preferred to shear- reagent grade oxahe acid crys:

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

Test.

Sheanng cold works adjacent metal and af- :ll$O) to 900 ml of distilled wat: 1 2.2.1 Each recommended practice con. fects the response to subsequent sensitization. until all crsstals are dissobed. ,

4.5 Erc5ing Conditions -T >

s tains a table showing which classifications of Microscopic examination of an etch made on a specimen should be etched at 1.

} etch structures on a given stainless steel grade specimen containing sheared edges should be are equivalent to acceptable, or possibly non- made on metal unaffected b3 sheanng. A con- mm. To obtam the correct curre acceptable performance in that particular test. venient specimen size is I by 1 in. (25 by 25 4 5.1 The totalimmersed are.

I Specimens having acceptable etch structures mm). men to be etched should be square centimetres, and 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 Specimens hasmg nonacceptable etch struc-

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

solution. found.The boidrace si ihe numbers end or these refer io hiersture recommended pracites references !

7

]

i k

l '

i

) m Y

I h r~ M a

i sf i

i (b A 262 1

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 men m square cennmetres

' surface ftnnhmg should be performed as is hsted m TaNe : 4 6 &chmg Precounom required to remove fore.gn material and ob- 461 Etching should be carried out under on gradet such as 304L.

tam a standard, uniform fmish as described m j rested af ter sensaame a ventilated hood Gat w hich is rapidly 43 For sery heasy secnont specimens

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

range of maum um car- '

priare surface while mamtamma reasonable ment of osabe acid. is poisonous and irritanng l hese senurarng treat. to mucous membranes y l  ! hetore the spet:mers <pecimen sue for consenre-r resorg Ordmar-I :h remosal of more mateful than necewary 46: A y ellow- gree n fdm ts gradually ,

W wahc acid e'ch res: The formed on the cathode Tha mcreases the l I

nsnamg 'reatment n i el base htfle mtlue ce on the test results p i Howeser. m the speual case et surf ace car- resniance of the etchme cell W hen tna oc- E

! 1 curs, the fdm should be remosed by rmsmg l Nraat on i so m e n m e s ercourtered tot m-wnte. in tubmg or castmgs when lubricants the mside of the stamless steel beaker (or the

-[ ]

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

Currem - Hauery . 30 c'c H N O:

capanle of supph mg are employ edi it may be possible by heavy '

i pndmg or machming to completely remose 4 6 3 The temperature of the etchmg solu-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

' alternanng two beakers One mas be cooied I ndr: cal pie;e of stam- Wertaken to demonstrare such effects 4 3 Polishmg- On all types of materols m tap *ater while the other is used for etch- ,

a 1-w Io hhrre > craw secner.al surfaces should be pohshed for mg The rate of heatmg depends on the total ]

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

• elds should mclude base -

rire . w eld beat atfected zone, and weld kept as small as possible while at the same I

'm mre - Fo r e s a m e time meermg the requirements of desiraHe metal Scale should be remosed from the area - '

actures at 2 %) to $4iG mmimum area to be etched to *e etched. bs grmumg to an 50 or 120 grit 464 Immersion of the clamp holdmg the k Edm ( e n fMh on a grmdmg belt or wheel wahout a  ? u The etcessne hearmg. and then polahmg on suc- specimen m the erchmg solunon should be ,"

"ade me r de. and asorded e%eb tmer emers papers. No 1. '

a pm c t't na m ess and 4 ? Rmsme- Followmg etchme the 3 pea- .

men to ht eveJ w or tmer ihn pohshmg operanon men should be thoroughly rinsed in hot *ater can be carr:eJ out m a relatneh short ome )

and m acetone or alcohol to avoid crystalhza-a6 M e il C 0, smcc all farve scra:ches need not be remosed ( l4 weet E  %'ereser practical, a pohshed area of I cm- tion of osahc ac:d on the etched surface dur- 9 soi o nen er mg drsmg l more n devraHe if any crow sectional ^

Mewon n few than I cm. a mmimum 4 8 On some speamens conrammg moh b-ea e aj ey of I cm should be pohshed W hen the denum t A!SI 316 316L. 317 317L) which ,*

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

\echen should be used may be difficult to rescal the presence of step mmens

,e r44 &chme Solunon - The solunon used structures bv electrohtic etchme *rth otahc '

TI acid in such caset an electrohle of a 10 "c

' referred to shear.

l ow carNo er a des reJcent etchmg n prepared by addmg 100 g of

g g,,g m craJe m osahc aaJ crsstals (H;C O.

solunon of Jmmomum persulfd!e. ( N Has O..

mas be used m place or osahe aad An erch

] 4.

( :nt metd md d' "hl all rutakmlare of dantleJ a.ocr and stirrmd -

l .cn r sc%raanon Jnsobed of $ or 10 mm at 1 4cm m a solurton at Y in em m ue on a 45 & m - T he polnhed room temperature reaJih deselops step struc s

tures on such speam ens edecs sho udse r ,

she.irm \som

%n 4$

To obtam the correa current dene 5. Cimification of Etch Structures g';

I* '2 g h 2'  %

to be etcheJ should be measured n ,

($ '

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

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

M'ed untd the ammeter readme m amperes n

= .

_ 5: The etched crowsetnonal areas should [

y

) 4.

A AJ N $?

-/ W.i W- -

+,

N &* s

.a'.$.'ya M-g . . _

• x-h A 262 I

I p 4 l*rm tu r l

detected by pronounced disches  ; y n a 4 h tes be thoroughly cxammed by compicie trascrse 5.5 Some wrought spvcimens. especiall) ! acid and 3 % hs from inside to outside diameters of rods and appheaNe ont tubes. from face to face on plates and acrow from bar stock, may contam a random patternI all zones such as weld rncial, weld-affected of pits.11 these pin are sharp and so deep' grades of auuen zones and base plates on specimens comain- that they appear black (Fig. 7) it is powbie I 316L. 317. 317 that the specimen may be susceptible to end. biht) to intergr ing welds, 5.3 The etch structures are clawified into grain attack in mtric acid only. Therefore,i chromium carb-esen though the grain boundaries all hase detect susceptib

- the following types (Noic 2): sociated with sy 5.3.1 Step Structure (Fig.11-Sicps onl> uep structures. specimens haung as much or more end grain pitting than that shown in sion. w hich. so t between grains, no ditches at grain bound- intergranular at aries.

Fig. 7 cannot be safely awumed to hase low 5.3.2 Dual Structure (F,g. 21- Some nitric acid rates and should be subjected to enuronments the miric acid test wheneser it is specified. 6 5 Prachte l ditches at grain boundaries in addition to steps, but no single grain completely sur- Such sharp, deep pits should not be confused sdfuric Acid 7 ,

r with the shallow pits shown in Figs I and 6 solution contai l rounded b) ditches. scc* corrcr si.

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. ular attack mo 5.3.4 Isolated Ferrrre (Fig. 4)-Observed 6.1 The use of these classifications depends on the hot acid corrosion test for which stain- chromium-rich in castings and welds. Steps between austenite susce ptibiht3 14 matrix and ferrite pooh _ less steel specimens are being screened b) etching in oxalic acid and is described in each ated with sigma 5.3.5 Interdendratic Driches (Fig. 5)- Ob-of the recommended practices, important both of uhich h served in castings and welds. Deep intercon-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 Acid Test is a 120-h test m boihng 50 "c CEPTIBILITS with some shallow etch pits at 500 ~ . (Of TACH 1% ST solution which detects susceptibility to inter-importance only when nitric acid test is used.)

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.

test is used.) less steels (316. 316L. 317, 317L) which is h ferric sulfate Nou 2- All photomicrographs were made with known to lead to rapid miergranular attack 3) which meas specimens that were etched under standard condi- less steels to i tiont 10 9 oxabc acid. room temperature 1.5 min onh m certain nitric acid enuronments. It 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 sulfuric acid test does rescal suscepitbihty completely surrounded by ditches in ever) 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, crackmc termine if there are any grains completely 6.3 Practice C-Nstric Acid Test is a 240-h 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 ,

microstructure. This test also reveals suscepti- carbides m tess prominent than those on wrought matert- steels. It doe als, or are entirely absent. Howeser, any sus- bihty to end grain aitack in all grades of stam. t ceptibility to intergranular attack is readily less steels.

4 w

A wS e

I g-9 .

s.

a

+g. .,

i

'h, A 262 f 6 4 Practice D- Naric H drof7uoric 3 Acid tergranular attack associated wuh sigma phase i Test is a 4-h test in a solution of 10 C*c nitric in austenitic stainless steels containing molyb- 3 nced duches acid and 3 c*c hydro 0uoric acid at 70*C 11 is denum, such as Types 316, 316L. 311 and }

ght speamens. espeaalk g

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

is are sharp and so Jeep grades of austenitic stainless steels ( AIS! 316. Non 4-To J tect suscepnNhn to imergranu- f 31el. 317. 317L) and detects only suscepti- lar aitack associa.ed wien snima pnase in auuenaic p r ack (Fig ?) a is posuble 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 3 ric aad onk Thererere chromium carbide precipitates it does not 7 2 In stabihzed stainless stee!. Type 321

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

• i fand perhaps 347) the terric sultatemalfuric 3 amens hamg as much or itfire than that Oown in soaateJ with s:gma phase or end grain corro-sion, which so f ar. are known to feaJ to rapiJ aad test deteca suscepnbdin anocated anh j ~

preopuated chromium carb des and with a .

itch issur ej to hD e lo* mtergranular attack only in certain mira aad .e

i' d Ih*C

• h'ch me be insi W e in the 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/

solutio n contamine 16 "c sulf unc aad and a shown m Fres Iand^ ~

^cc copper suHate with the test speamen corded as-receised material it mn also be used to check the effectiveness of stabihzing f ,

embedded m metadic copper shot or gnnd-utture C!nuncation, columbium or titanium additions and of re- g , ,

ings, which Jetects suscepobility to intergran- ducnons in carbon content in presenting sus- ,

'ese classifwanons depends ular attack assoaated with the preapitanon of cepubihty to rapid intergranular attack lt .T rouon f eu Mr 4 hgh vain- chromium-nch carbides it does not detect may be apphed to wrought products (incluJ- I 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 treatments at 1200 to 125WF K50 to n?5'C), 4 PR \CTICE B - F E R RIC SL L F -% T E 5L L- which is the range of maumum carbide pre- M w

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

FL RIC %CID TE5T FOR DETECTING 5Ls- apnarron The length of time of heat:ng used p i ich test m Nuhne 91 "

CEPIIBilli) TO IN TE RGR sNL L AR \ T. for this sensitizing treatment Jetermires the g

ca suscernNhn to mrer- T Rh IN si stNLE55 $ TEEL 5 m N maumum permnsibie corrosion rate for such

! s sou a:c a premanh aan grades in the ferne sultate suitunc aad test } .

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

E.

5 ternc sultate-50 "c sulfuric acid testlNote PL. T I ' it 'Li w ngh is h w hich measures the suscepnbihty of stain-L Rapid Screening Test { y rapid imercrandar attad ten steek to intergranular attack The pres- 41 Before testmg in the fernc sulfate sui '",

'nc aad enuronmenn ir func aad test speamens of certain grades of r acePhNhh to end gram ence or absence of mrergranular attack m this - -

'eM is not necessanly a measure of the per- stainless steels (see Table 31 me be gnen a No founJ onh m certain  %

tormance of the matenal in other corrosne rapid screemng test in accordance woh proce-ments The terne sult ue. dures gnen m PractNe A. Osahc Ac:d Erch 5 -

emironmenn The test does not prouJe a Joes resca suscernNhn Tesi for Clasuficanon of Etch structures of ,,

cmaMc Mne sonsotuent  % for preJKring resntance to forms of cor- '

• twon other than intergranular, such as gen. Stamfess Stech Preparation. etchmg. and the w s:ce's TISI 121 and g- '

eral cor rouon , pit t i n g or st rew-c o r ro3.o n clasufKation of etch structures are desenbed ,

crJdmg therein The ne of eten structure es aiuanons

\aN bei leu n i 2 4+ L h )

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 d inh rerandar aitak 3 mou y,propnje at twe ses er al 'eu meMmds mda- Jad !csf a st'eaneJ m Tarie 3 4 1 1 Corros.on test s pe u m e n s ho me ac. ,,

• #f-mum carNde preurna'e h *' J i"J ' "' "I 'IC' h' s t ad e s o f " J o c " -

veet ceptable etch structures in the osabe aad etch i phec prnirnaic 1 hc 5 II The terne sulf ate 4ulf ur c aad test test will be ewennaih tree of intergrarular l Ed ' '

J m n% Nk numhearme  ;

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

aNctated woh *he preapitation of chromium Such speamens are acceptable without res*mg ,

na ut he s n.He m the I CarNJes m unuaNh/ed auuenitN uamiew m the ferric sultatenuif ur;c aad test AN gec hu ao re s cah suw e pt,. '

'.. 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  : &, (W[. ;

y; DC NM s-

[9I"w '

_WW

,Jv M.. .

ye '%.

~

. ,. J. -y

(

l t

h A 262 l

must be tested in the ferne sulfate-sulfuric Erlenmeyer flask. 11.4 All surfaces acid test. 10.1.3 Then measure 236.0 mi of reagent '

in edges. should be I

' grade sulfuric acid of a concentration which abr.i w pa

9. Apparatus must be in the range of 95 0 to 98.0 % byf used, poinh slow i

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

Fig.8. slowly to the water in the Erlenmeyer flask so. 113 All traco o l 9.1.1 A four-bulb Alhhn or Soxhlet con- avoid boiling by the heat evolved.

I ing heat treatment.

denser with a 45/50 ground glass jomt. Over- Norn 7-Loss of vapor resuhs in concentra" " mosed Any wale ' i alllength: about 13 m. (330 mm), condensing of the acid. s gnndmg, for es 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 must be such that the cradle will fit the 1%-in- is dissobed (see Note 7)- naied acents such I

' (34-mm) diameter opening. It should hase .

then we'ighed to th 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-9.1.5 A sibcone grease 3 is recommended sentmg as nearly as possible the surface of the ; there is an apprecia 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 12.7 Addinonal l ployed) it may be possible by heasy gnndmg l or machming to remose the carbunzed layer hase to be added i

10. Ferrie Sulfate Sulfuric Acid Test Solution completely Such treatment of test specimens sion rate is estrao 10.1 Six hundred mdhhtres of 50 '~c (49.4 by a change in the to 50.9 ("c) solution are to be prepared as s not permissible. escept in tests undertaken to demonstrate such surface effects. ferric sulfate must go;;o g loss of all specime 11.3 When specimens are cut by shcanng.

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

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- The number (3 or 4)is hmaed 1

' ncentratior; whicb "

e U" '

'5 0 to 910 "c by J ' e

• e Me is used, polish slowh to asoid overheating t e acid, +-

Sand blastme should 'not be used

- 13. Calculation and Report [

rfenmeser iflan 115 tolt All traces of oxide scale formed Jur-ing heat treatments must be thoroughly re- 13 i The effect of the aad solunon on the t 1

Jts in contentrat' "' material sha!! be measured bs determinme the r -

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

bs grirdirg. for example in stamped num- rates should be reported as inches or penetr e bers. must be remosed bs immersmg the spec- y ,

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

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

Innes per w,m h = < y a,a4 ~

mf" thC dai gahars acam anJ s msequert actn anon m ai -

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 tool espose) area calculated l b '"

11 ' The specimen should then be Je- 'E all fernc suMate g greased and dr:ed usmg sunable norchlori- for chromium nickel steefs. J = . 9 g cm) ' -

nated agents. such as soap and acetone and for chromium-rickebmohhdenum weels J= 4a 3 Un g cm 4 1 mens then weighed to the nearest 0 H01 g .

a total surface 12. Procedure Nort s-Conseruon factors to other comme

• a mended S pe ci- used unas for corrouon rates are n fodo*s h 12 1 Place specimen in g! ass cradle and im- '"'"N*"*'I "

'"# PI

t be cut so thar '"*'N"""** """M }*

• merse m boilmg solunon I - P" " "

I width of b ae incnes per moneh = 12.000 a mas per scar 5 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 Jenn = cam per

1. '""M "I

• C wou!J result in corcentrar on of the aaJ If ware me re ner Sour ,

there a an appremNe chance m the lesel. the i no in = $ 45cm; c h sum h surtase test muu he repeated wnh fresh solunon and a ,

s is reared r ,

" PR ACTICE C- SIT RIC ACID T F 51 F O R D E- 32 a e obram a stan -

I. L onnnue :mmers,on of the speamen T E CTIN G s L SC E P TlHit. li ) TO IN TE R-  ; ,f.

'#" E."r vers GR O ugR griACA IN STUMFw Mr a total of 1216 h. then remose speamen. 5TEFIs  %

^

'ouM be ma. '

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

' P'" * ' ' W e from or emal weight p

)rdmarih . re 141 Thn recommended practice Jescribes '

necewm wm 12 5 No miermediate weighings are usu- the procedure for conducting the boihng nitric  ;

"Ih HO*- :h necewars The tests can be run wohout aad test (3) as emplosed to measure the rela- '

m'erruptmn for 120 h However, if prehmi-ice cathunza

• '""J"" # %rs rewits are desired. the specimen can be tne suscepobiiny of austenitic stamless week to intergranular attad The presence or ab-h '

remosed at ans nme for weighng  ; ,

'M or Nrder' sence of mtergranular attad in ihn teu n rot

• 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 n s ermJme the material m other corrous e erwironments. iI iunted !ner 12 ' -\JJinonal terne suit.ite mhiNtor mn m parncular, it does not provide a han for 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 eJens cJ other than mtergranular. sucn as generai cor-h 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 [

o 14 2 The hoehng nitric acid teu mas be i j.

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

' nnht J % .

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

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

'Jv reCen eJ mater:Jl It n Jho somenmes '

(;

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.

• 7 l '

[g. ,h m

e* =? ,7 '

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

u.p . m h

I

• y n,. L ~  % s. - . .;.. .

% e b

l /

' p3 ' - . * '

, ~

d'~4. , ,s

]

t

• (-

^

[ '- , %

l p

-_ s5 l

gYg- + 1 = '- -

? \

l h A 262 1

agreed upon between the surpher and purchaser

in preventing suscep

ilii) to rapid intergran- p, Preparation et j ular attack

• One of these consists of a one-hire Erlenmeyer flag I 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 associated with one or more of the followmg: (J) results obtained with a reflus condenser tend to be rnus t be considero 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*

container is the so called multi-sample testing appa.. o( test solution ti mg grades, and U) c;ma phase constituents in I staoihzed grades. The tuling nitric acid test should ratus (4) which was designed to permit the testing of maximum conseni not be used for extra lom carbon molybdenum- a large number of specimens simultaneously by pr* about 100 g Sp l viding for replacement of the acid in contact with

! U bearmg grades unless the matenal tested is to be 5hould be cut so tt j used in nitric acid serme. See Practice A. Omahc the specimens several times per hour with redsstilled Acid Eichmg Test, for information on the most acid. Because of the lesser accumulation of corro mm) width of base

' appropnaie of the sesersliest methods available for sion products in the testmg solution, the rates ob- side of the wcld I l

iC .f' the evaluation of specific grades of stamless steel. tamed with the multi-sample tester are consistently lower than those obtamed with the conventional b.ir. wire, and tut 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*"he fe' esul [ c compaUed d recN), it Ys subject to end gra bide precipitation. The length of time used for essential that the same type of apparatus be used for proportion of en this sensitizing treatment determines tN: max. all tests. should therefore t' face is actually ro t imum permissible corrosion rate in the nitric 16.2 Specimen Supports- Glass hooks, acid test. The most commonly used sensitizing ing nitric acid. WP stirrups, or cradles for supporting the speci- 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 posed to the tota tested in the same container do not come in tubes), castings, and weld metal of the various stant from test to contact with each other.

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

grades of stainless steel (Note 9).

solutions and of keeping them boiling should be propor-

15. Rap,d Screem,ng Test the exposed cros?

i throughout the test period. An electrically 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, 16.4 Balance- An analytical balance capa- Prior to testing or as given in Table 1 may be given a rapid 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 the sheared edge Classification of Etch Structures of Stainless 17. Nitric Acid Test Solution machining or gnn Steels. The use of the etch structure evalua- 17.1 The test solution shall be 65 : 0.2 IS.4 All surfac tions in connection with the nitric acid test is weight % as nitric acid determined by anal).

sis. This solution may be prepared by adding ing edges, should specified in Table 4.

15.1.1 Corrosion test specimens having ac- 1 0 grit abrasise, distilled water to concentrated nitric acid (re. is used, polish s ceptable etch structures in the oxalic acid etch agent grade HNO3 , sp gr 1.42) (Note 11) at Sandblasting sho.

test will be essentially free of intergranular the rate of 108 ml of distilled water per litre of attack in the nitric acid test; such specimens 18.5 The inter concentrated nitric acid.

senting as nca@

are acceptable without testing in the nitric Nott Il-The mtric acid used should conform .

to the recommended specifications for analytical material as it will acid test. All specimens having nonacceptable 3 reagent chemicals of the Amencan Chemical Soca- surface machinir

, etch structures must be tested in the nitric acid 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>

Arsenic, man. % 0.000003 should be machi 16.1 Container- A 1-litre Erlenmeyer Chlonne, max. % about 000007 flask equipped with a cold finger-type con- Heavy metals. max, % about lead 0 0005 priate surface w denser, as illustrated in Fig. 9, is recom- andiron 00001  ;

specimen size fot In addition, the fluonne content shall not exceed dinaril} , remos a mended.

Note 10-Two other types of containers have 0.0001 % and phosphate (PO.) shall not exceed , essary will hase 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

t8n se en sno., me 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-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 g o The se:und %;se . , '

f acJ+es 'or accurate Ae+R5:rg Ird the solume h e J s '. 9 or ma&ru'g N rem e > % -

,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 ss - e,es m m 4

I re r?:f "

• e "e s f " d ' 1' TdI'T U 6'

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

• IC E I e ' 's ,, o, .eu y ' e. , s, c '. ',.m^,,, - y m-e m m c- ,- , oo , sre e s coc e r, .e. cer - :esa ..raer se- m :e ~ sure f N 2cm m . .m Ur e ,

• • >C

.eam.e ,,e.ur ,- ,I eas e cue '

e t -

z

; ~ ! " re - e'ai s "i Red 7 e Pe-I"'I"C"'" I "" "' " 2 "

- e mes . a ,,-2 ..m,e = -

em- ' -s

- , e me . e -e- - -

seraIe 's s5 t' I 5)e A e -4 h

{ y , , ps L.II u.

p ,s

_ e s [1( a () N6 aid'(

g, i9 : 'f '"e !a4 1rea e a re se" f e J "N ' '" e e g . U ' E ' ' C U

, .w... .-e: . -e. - n. .e ,e .ec re - ,

, an he s eh af y 'ur: v= -e : cJ xe: m 8uwe ~ n

a. .y ., c , , . I' a"ca t 9 'be4 If odWIS

• as he "dICJ d d "I " " l' 'U d I $ J JE0' " O I \ ' 'I U 1.' s r he r

• e g"e d !o P e

, . f ett t #L'

• W Sfd II'dE" r nt!rs aad The e a reu l 4 rnr-e 2sm , ; cropona> or e-a eram m +e wear e, i

'see P "

!"e r e'stre he k ef' t7A grie%g sysh sLF sht'4

\n g ]Yke ;dgjrirg ; y p 3 r .* p e.r jeg A gy 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"

. ".e ".e-c. N 'ef ec e~ .e n "

I .N)r fi r 2 'he Spec t - i "i E d' d 'IO E ' f \ 'l w . rJ osr ewe -

$N 1 Ih'd' ;4,'p,

, ,. - [ f s r 1 ' *' ' a )

I ersea ar ai i m e .. es are "eme teved ' researa inseu p v 5.c J hs r s - g

' arw e r:

• e c , os +e case a sm m a ~ er ,

J lpj! spe; ; mens 'I s 'he raf.'1 <if'"e$ l'ss-SCC it'r Jl ar e a e t - ' A'3 r % If -~ " e " s *"45 L a " " '" "f ""'f"e^'!* '

I r do 9tJf Jlme :p U' M w, " ' ' I N 3 ,- IIed

• h ' ' u *, ,, e E e U N * <eurf aced 'n 'Pe n.de !i s des ra'e 'a re ae r

. i., p 7y.,,m j, sIaD' ' M Fes[

,.,,,,"5 ** '9 o ' ' r 2 " ' ' N' 3.

't) IesI ht r ;Isfed t1in Iesfs g A4 ' ,4 { g 4 m, g pgskg g ,q g y 3,37 gg + p l

r heatre the es 'rea ~ e"s car ir"~ Nrs Aires or tubes De Nrrme d '"ese ' ream e-S sM

pem h, q j ; p L. At d * * ' p r 'pi . u m e. 4 ' 'ha! 'he areas of

.eFe C 4r'.ev n , . " , + 3,'

's r 3 - ., e - r a ,' ,. n n , %e h

A ri eier' r , 3,? as. -^

'e ; *s ac re2.'J r 'e j e "i "e'*

C e1[' 'W J C r s Ws i'rN A"aI! 9til esCee ! aw t.,3, .,

1" -

' ,3 e.gc j7p3rg-, 3g .=* s,, me its 'er tha o " P ? "" ' "E e t r t l' e l a f '"e Te '" e " re " e '

sreca: er rea e m sce; ,e,

- d ' e f .s + cJ" "P 'eV g

, , , i, .4 i

al ba A ;g, a s .se *Te em *N9 s, _ . , , ;, , x , .g..g ,, e 3

,,, - m ~ ^ ' , m" c-o,r *,me e a

,y , , m y , ,, , y y g g, .g,. L n we. , m . .m . _ . _ m,m g

e are w ~, , rear ,

i

., e,c, ,, , ,, .,, i

, e rear < eues um -e rermisnea m ,_ ye , m i sd he 6 4 - 1 ; m h w. or gr rd re pr or to reu:rg ,

e ., . g

, s ,e; _ .

j l rntned hs a na!s - }9 E SAI5dfJbC\ f Ihf S IU C

• e 9 l f' d ! lld '

l rared M MJme +eeJees shoa,1 he hrisned are No m or 19 Proc edu re i

i d notic m a ire :o er.r m e. e parer a on w rasne rarer D

( ;2) INore 1i i e y ne! rom 5 slo w i s to asord osernea'me is ne3 u,;em y,.s . .s e nor A 3 i 4arer pc- re ,o SarJ % e s hou'd "orhe useJ 3c , , ,, , , ,ug .s e ge g ,., e .,,, f .

p ,

s< The wer: 4 e teu a srec ~en rerre- g pnm a 3,m m q f 3 ,;;< w ,,.,,- 1 l .

m'-rie'geu s a mi . e Nor 6 I

s h. -m d s or br, " f i r'i a " c a r j s j% p. m i c k ! " e sur be t'f 'he e e au @' O m or yao o gese , , J s,3 g . moi gm. ;3 3 3e g ,1 .

N l

m e i r ms a

• ol "e aseJ " serw e Um s suc h ;g _ p, e .,c c p, x , , .a ,e 3 y. p p 3. e ,

'( ' ' '" a % >

Nr%e a m"e sno ud he performed n% gi .-

g , 7 ., e ,, enn .eu g . c-  ;

'tr i.

• ew rcJ m re m e u re r m e er m r a o n- s 4 -

'am a cart trj 2 n f. r m l < r e "# 1

' " * "# ' ' ld r

.s s Wei fle d : P

."y ' ~ (

• 4 F.'r er. *en s ses om s pea me m h

e' e%f .t s " 2  % s%'*Yee  % *e %a

• e P s *

,r,3c, 7, ,c. ,y .% g 3 7 e ,y e m-. -

A w.1 he w n+cl to re;'rne"t t h e g p r o-grade 2 W6*.2 sbc ors reu :ne, ern.

1 9" '

?nre urtase a ni e mau'am're reau mahie "' if "f d ' ' ' Tf ' " * ' ' f ' C * 'f

(,

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

• e s!'" g ()T

_""N" m .,; ,

r mre eu a s-e, ,

n u- ,ue. >

' "a rm remmal of more exeru '*an p ,p ,,,, ,

.,,g .

s_*,

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

'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 +'N

Isa!!s 41'5 t Fises*r si rr s ' e ~

• e c ' e ,' ' ed f1 b.

fli1* e s e r . In '

• e spec 'al J De tr % J r. , ,,, ,, , , ", m a , q '

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.

5- .m  ;

<d &O)s Q5 W 4

h *

-- -W a w ~.

• u:% ges 4  ?. e . p : yy

. y ,_.. . . _

• j .g"N Jr7 7:te :*tfv

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 19.3 After the specimens have been placed where: not proude .

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

through the condenwr and bring the acid to a A = total surface area, em . 2 such as gen boil on the hot plate and then keep boiling W = weight loss, g. and C0"*' "#

i' throughout the test period (Note 15). After d = density (Note 18) of the sample g/cm' .

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

water and treat by scrubbing with rubber or a monly used umts for corrouon raies are as follows: anack anm 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 inches per m nth x 8350 x densit) = milligrams tergranular i mah be facilitated if desired, by dipping'the 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 Nott 15 -Care should be taken to present con-212 The i

~l 1.guarein 8metre

= 6.45per cm-hour j tamination of the testing solution. especially by flu- acid test mt 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 the same hood with nitric acid tests.

, , "'"I reduction in AISI 304. 304L. 309. 310. 3:1; ACI 79 ceptibility to 19.4 For most consistent results, the test cr.s 316L and 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 umulated seruce ies for nnne acid seruce specificall3 rather than as an carbide prec procedure the rate of attack in the third period

' indicaior of relatise susceptibihty to intergranular corro- heattnc used should esceed that in either the first or second 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 monly used periods As an alternative, when the test is bemg 202 ReEort- Results should be reIorted 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-for) performance in three 48-h boiling penods with PRACTICE D-NITRIC HYDROFLUORIC u

~~ 37 '

ACID TEST FOR DETECTING SUSCEPTI-fmal acceptance being dependent upon satisfactory BILITY TO INTERGRANULAR ATTACig The maten so, b IN MOLli BDENUM BEARING STAINLESS tested in eac pc ual agreement a cornbi at of one 48-h penod and two 96-h penods (not neces. STEEI.S (63 ment: (1) sarily m that order) mstead of five 48-h test penods may be acceptable for routme evaluanons. 21. SCOP'  ! nealed)and 1900 to 200 NOTE 19-See Pracuce A for mformanon on the

20. Calculation and Report most appropnaie of the severaliest methods asatla- Suenched f

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 -

? ,. s, :,y u ~; 2092 .

neun

• Y> y..

o r 5v

. n x

• u m

, "3

~ ' .

, -- -m .

m

- - .Ar#

~; *

,Y T,4

3

- g,:

r i

A 2

l

\

p

@ A 262 t @

I  ! ~ .

^'

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

u ,

N i measure of the performance of the materialin the basebre spec; men isee foorrote c of TaNe ~ 'y.

n t, a a ,

aiher corrosne e nironments The rest does 5 ). ' Q 4 h7A[

not proude a basm for predicnr2 reustance to d

orms at correw other than ntergranular 23. Rapid kreening Test , 'T'L

)

l c h as ee,erai cerrouen put rg. or strese 23 i Before tesnng m the in 7 nerie 'c 4g *'

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

w' 21 . I The li m mrrs 1 ~ hs dron e ric :ess steen as gnen in TaNe ? r h E < .- V-n w eene a f q wJ 'es detem s 2 s e;'t h a mfergranular rap'J screermg test 'n accorjame aan prece. _ ' ,s-4 res m 3

=

... r k e i+

203a 3 NcJ t e d dah the preapaawn of I -

1

%s Jures gnen m Practse A. Otahc AuJ Etch {e/

h. r o m u m car N es m moi.Nesm nearmg , .

M'

! M% C stamiess steen i Ts pes 316. 11' 31^ L. and Te st for C!asufication of Etch Structures of Starricss Steels Preparanon, etchirg and the f

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

mm = wm .ergran Jar an.sa assoaan J e sigma phase classificanon of etch structures are described $' -

~

W

• n te'e ume !s pes of staHew steel therein The use of etch-struc*ure esalua'rons v. .

nun ,m3 #

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 >,

crrown c a ." ceptJNe etch structures in the Otahc AaJ p.

iTspes ilh and 31' stainless steel) It mas i

Erch Test will be largeh free of mtereranular also be used to check the effectneness of 1

b

\

g " '.' attack m the 10 Fe nitric-3"c hsdroduoric aad , Y. s rehcnon .n catho content in presentmg sus. i .f' test Such . comens are accepraNe *Hhout g \' cernNhn to rapid mtergranular attack iTspes resurg m the 10 ~c nuric-3 C hsdroduoric 1%

. 3 H et and 31'L3 It mas be arpheJ to g .( g ac J test All speamens hasing nonacceptaMe '

t C 4roueN prous i.nWJa c ohes t casungs. etch uructures must be teueJ .n the lii 7 - } p' %

trd *e:J m etal aric-3 7 hsdroduoric aad test -  %

g4

. .1 s

\;'e a m e ns .it estra hi* tarbon graJes - ~@J + -

i T pn 11

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

, ,q M,-

~:

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 g,;

, [. (($ M C'T>

• Neh n the rJnge or matimum 4

eare. % ,r carmde preep r 2ron The teneth of nme or 24 1 l TeJI Gimder! I hore 2f'l- The tests Q, j y@ p[,

" 4P / " ' -

• ' "e if m d used f or :5n sensdizmg treat men t

• dl are conducteJ m cs hnders of poht s msi chh>

ride ) (P\ C) as shown in Fig in The test p' "$(?

Rereraih he ore or two hours The most com. cshnders can be made from 12an (305 mmi I I

J be re pone ' "T

) wh used sensavire treatmerr n 1 h at lengths or l'+m Pk C pipe t ' +in l ell as !F e ner 129 0 mm i *aH p hy enher of the tcHo* mg r*o tech-14 's .

S

• d ~* r l crmds r niques ill one end or each PTe teneth n l 22. Summars of \fethod piu eJ *rth a dai of ' m n P\ C sheet and

,3 g [Qde

.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 i gg g n gg g t he mrerial submdred for esa;ar on a hiler rod. or l J ) ore end of eac h rice ieneth s

[ j(-

!s e %I stNi t w ;n . % "( 9

'ev ed n each of r

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

• eldi n g a 1 cin N PS I

9 eat i/) avreseneJ # comrren ab an- (hheJule 401 societ-npe PW cap onto the

p g);

i  ; T<.

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

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

• yer 6

.. . v me-% g e .', g n e ; 24 1 2 SfecWe" Hour'T tN ote 201- T"e A speamens mas he suspended < n the test solu- {t 3,'

te e 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 d' g*

$lf.,

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

'c u Je%ribed an thn paragraphi or a TF E Ouor.* * " * "'

I 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

'e ..'( 2h i'

..c a r me n t (!) a sers taeJ spesimen and 4 J , JriheJ m one end of the speamen The spec .-4 s J- / e.

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

• e a s-

)(.

h,G. ?< ?c' d 'e" e e t men heade rs rras be m ue m c'ther of *o -

,n.o m- re e sea umma ynem yye., .ns if,a i. n ,23.m y :ewh at n E. Q,-

, , 4. a$. -

3 '"e b ret e n cJ gee me n a vs no r 3 hi> 4 a C u.)rocarh m t ubm g i l-in in s de Jia"'e t e r s a

• M ,3,QQ -.

{,d .

i 4

o

• K... wg . 3t - t ap - . . ,

I

,# j j;

' *c#M A dj "

, t

@O[ V)KhWD. M N .b b N b b

.c..y . f* w..n . . .s , , ,a .',* ,,

p a .. ,

. - w , .

~

2 g~ g y

, m i R r.

h A 262 25.2 The intent is to iest a specimen repre. portion of si to dnlled at one end to accommodate a %-in. that sampic e  !

senting as nearly as possible the surface of the (4.76-mm) TFE-fluorocarbon rod. The hold- footnote c of h ers are flattened into an elliptical shape which material as it will be used in service. Only such 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 l

with a hammer, or (2) a %-in. NPS (Schedule dard, uniform finish as specified. For ver) heavy sections, specimens should be ma, mater bath unti.

80) socket-type PVC cap is machined to re- rneasured with a duce the outer diameter of the cap to 1% in. chined to represent the appropnate surface while maintaining reasonable specimen size- Nort M - 88

! (27.0 mm). Holes % in. (6.35 mm)in diame-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 Nort 20 - All poly (vinyl chlonde) maierials Pl oyed),it may be possible by heavy grindmg and acetone, dr 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 the sheared edges should be refinished b} taneousis the obtained by placing the PVC cylinders within '

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

25.4 All surfaces of the specimen, includ- for each maten The temperature of the bath is maintained ai ing edges, should be finished using No 80 or 72 to 73 0 to offset the low thermal conduc. 27. Calculatiot tivity of .he poly (vinyl chloride). 120 gni abrasive paper. If dry abrasise paper 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:

25.5 The specimen should be measured of the tuo spec 24.1.4.1 Caution-The 10 % nitric 3 % and the total exposed area, including the inner measured bs de hydrofluoric acid solution will cause severe surfaces of any holes. calculated in square the specimen.

burns if it comes into contact with the skin.

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.

l ml of 48 % hydrofluoric acid (sp gr 1.16),and imens, one representing the as-received con. 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 es aporation. oxalic acid etch test.) '"'"

• d S PC' '

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

25. Preparation of Test Specimens specimens, one representing the sensitized S'ned.

l 25.1 A specimen having a total surface condition and the other a base line specimen. , 27 1 2 Type l area of 5 to 20 cm2 is recommended. Speci- which is usually the as-received (commercially I

Sicel-The rati mens containing welds should be cut so that annealed) specimen. If the as-receised speci- spec sensittted 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

\

~

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

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

• 4 y l 4 K : . ,-f 'e f ~* ~ ~ f '"  ; ,. g t

p ., .. . , .

u .~y , ' <, . . , . .,2 i a, fr%5 ;.; - u: Tp

,'A Q.,

,,P * '8'

~

s m g,y dlll ,s- .s ft .-;-* .

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

'] g I

ns ,- . ** '

v - -- -

^

.ne ,,,

Jr.: . - ,% h f [' .[

l -

t

.a h A 262 r

.t a specimen repre-ponion of it to gise step structure and use 27 3 Sigmficance of Corrosion Rate Ra-that sample as the base-line specimen (se:

le the surface of the rios- A value of 1.5 or less for the above ,.

' 4

, seruce. Only such footnote e of Table SL ratios indicates that the degree of intergranu-1ed as is required to 26.2 Fill the PVC test cylinders with 200 lar attack in the 10 ce nitric-3 "e hy drofluoric -

and obtain a stan- mi f10 ce nitric-3 c hydronuoric acid solu- acid test was not significant A ratio of greater '

.pecified For sery n and then heat in the constant temperature than 1.5 indicates that significant intergranu-is should be ma-water bath until the solution temperature. as far corrosion has occurred in the 10 C'c nitric- .  !

l sppropriate surface measured with a thermometer. is 70 : 0 5'C. 3 C'c hydro 0uoric acid test @ ,A i

able specimen size \0M 21 -li 's important that the test solution Note 22 - Conversion factors to other com- 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- 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 tion by means of the specimen holders or per square decimetre per Jag inches per month = 3a 9 = denuts = grams per h' 'I f bricants or binders

~

I materials are em-string After a 2 h esposure, remose the spec. s uare metre per hour J( '

by heau grindin?

imens from the test, wash in distilled water 1 in * = 6 a5 cm2 p.

PR ACTICE E -COPPER COPPER SULF ATE. b

, ie carburized layer l and acetone. dry. and weigh Then espose the 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 ATTACK IN STAINLESS STEELS 47) @ <

g

.6 4 Test only one specimen in each cylin- L-i re cut by shearing, der in addition it is preferable to test simul- I k be refinnhed by 28. Scope j

taneously the two specimens representing 381 This recommended practice desenbes ).

i ' ' * $ each of the two conditions of heat treatment  ; -

specimen, includ. ,

ch matenal paluatd the procedure by which the copper-copper a k,

, :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 g

~ used 271 Calc:darton of Indardoal Corronon absence of intergranular corrosion in this test h. .

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. ;

i ncluding the inner 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. [,,'

enches per month (Note __). based on the 4-such as general corrosion. pitting. or stress-i uld then be Je. h test esposure. is calculated for each speci. -

y w-

• l uttable nonchlore- " "#"# "E men as followt 28 2 The coppe r-coppe r sulfate-sulfuric I N I and acetone. and 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

));

. mens i = time of esposure. h.

A = area, cm 3 chromium rich carbides !! does not detect susceptibility associated with sigma phase ' ~

h ,

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

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 .

g the senutifed the laboratory-annealed specimen n deter-

• 'n ed rial of austenitic stainlew steck can be esalu-ated by thn test q

h(f

,e line specimen. I 2 d (com me rcialk 2' 2 2 Tsres JinL and 317L Stamlen Sterl- The ratio of the corrouon rate for the

29. Rapid Screening Tes ll .

j' K s-recen ed spec,. 7 structure in the ""I'/Cd 'P'C' men to the corrouon rate for 29 1 Before testmg in the copper-copper 'T "ators anneal a the as-recciscJ specimen is Jetermined sulf ate-sulf uric acid test specimens of certain Y M

- W,.Y ?

W.

aw

.-..'[z $ $~

ggp  % v y - ~

• ype @fgG s -

g g 1p

.. 3 k 9 5,..;

'm

(

, i i

h A 262 grades of stainless steel (see Table 6) may be 34.3 All aussi Nort 24-The solution will contam approu ccised" (mill an given a rapid screening test in accordance with mai g we  % of anhydrous CuSO. and It the procedures given in Practice A (Sections 2

• capable of meets through 6). Preparation, etching, and the 34.3.1 Specirt

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

.33.1 Electrolytic grade copper shot or heat treatments therein. The use of etch structure evaluations g in connection with the copper-copper sulfate- grindings may be used. Shot is preferred for sulfuric acid test is specified in Table 6. its case f handling before and after the test i

29.1.1 Corrosion test specimens having ac- 33.2 A sufficient quantity of copper shor '

[ ceptable etch structures in the oxalic acid etch 'E" d should be taken t "E.s is i be used to cover all surfaces 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 furic acid test. A!! specimens having nonac- an excess f metak coppu is present, is not , cartude precipiiam 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 I

30.1 A suitable sample of an austenitic reused if they are cleaned in warm tap water l completely imme stainless steel, embedded in copper shot or after each test. 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 qie si e n rease is rec mmended for 5' #

, 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 ;

cradle capable of supporting the specimens may be restrictions placed on specimen size b) 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 facem finish is to be evaluated. Chemical re- l may be remosed t throughout the test period. val of scale is permissible when this is the centrated nitric ac

32. Acidified Copper Sulfate Test Solution case. Mechanical removal of scale should be accomplished with 120-grit iron-free alumi- 36. Bend Test 32.1 Dissolve 100 g of copper sulfate num oxide abrasive.

(CuSOc5H O) in 700 ml of distilled water, 361 The test 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-1.84), and dilute to 1000 ml with distilled hol, ether, or a vapor degreaser prior to being the thickness of th water. Iested.

14 3ng

,_  ? :er ,

i e --

---

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

-p .-,--.yvw-,.,m,_ , , _ - - - - - , . -- y----w-_

i W

^

e - -

n gy.qy :.=: a -

N'~

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 ceived" (mill-annealed) condinon should be oser a smaller radius or through a greater e

, '4 .

sotunon wdt contain a ppro u-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-stabilized grades are testeJ after sensitizing tility, such as seserely cold worked matertal. a

} -

g haion 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 used Shot is preferred for 5 5'CL which is the range of maumum car- mine the maximum ang!e of benJ without h 8

,.{

hi de recipitation T he m'ost commonly used causing cracks in such material by bend:rg an ' l '4 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 as the specimen to be tested sh uld be'ta k en to as oid carburizin e er nit rid- y be useJ to coser all surface. the specimens The heat treat [ng n best 3h 11 Duplicate specimens shall be ob- 7

.n f

4hether it is in a sented glan

[rncJ out in air or neutrJI salt lained from sheet material so that both sides ed in a layer of copper shor of the rolled samples may be bent through a 1 ep i ,s the test as ~

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 side a minimum of 50 ml,in 3 (8 ml.cm;) of 3612 Samples machined from round sec- b a

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-

~

) ,

9 generaih specified in the The solution solume-to-sampie area rano n to "

~

are the two ends together in the s ne Heasy

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

apparatus dittates the finai 35 1

The rest spec:ments) shoulJ be im- (~

suitable desien An air or hsdraulic press mas . ~J ihe test specimen The spect- merseJ in ar-bient rest solution which is then also be used for bending the specimens

• L in should permit easy en "ro u gh t to a boil and maintained boilin? #

3h 14 Tubular prod'ucts shoulJ be Gat- k 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 ucts .

b 4-Norr 3 steasures should be taken to mini- 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 gg .

i7"

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

r 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 uared ' eJee n desirable on the specimens should be Fresh tesi solunon woulJ not be neeJed if the Fig 13) I bl 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 d 3 centrateJ nitris wJ at room temperature i lographic esammation of a longituJinal sec- 4 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 [

cumen should be JegreascJ through Isit dee and oser a diameter equal to , m]h.,a # 4 s Mr $mrai Pni. 3aL 5 hb [

h ent sus h as ateione. alco- .C

^

15e thn;k"cu of the speumen being bcnt nee va lii i or deceaser enor to beme , ,

4 t a i5 ,e U

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 % ,,,,

mg test solunon. A usual comparnon between ,,g,,,,,,,,,

peel" on the surface. mithout sccompanymg eracks ,,,g p g or fissures, should be daregarded also these specimer.s should asust m mterpretation.

a,nn :-The n=4ti REFERENCES (1) For ongmal descriptions of the use of etch Reagents. Specifications Recommended by j structure classifications, see Streicher, M. A., Committee on Analytical Reagents,' Am -

" Screening Stamiess Steels from the 24Gh Chem. Soc., March 1941.

(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 ---

(7) The use of copper to accelerate the mtergran. wnc Ac,d Tes ::

195, January 1954, p. 63 boa,cp wuno, (2) For ongmal dewnpuon of ferric sulfate-sul- ular cortouon of senutired ausieniac stainless 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 paper by Brauns, E., and Pier, G., Stahl und C***'**d'N' tc ' ,'

kranular tamiess Steels:Corrouon Reustance A Ferne Sulfate Acid Test," ASTM Bullerm, No. 229, Apnl Sulfunc of Austemtic Euen, Vol 75,1955,p.579. p, y ,,,,,d 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 I

acid test. see Hue), W. R., " Corrosion Test R., and Eisenbrown, C. M. "An Esaluation 3g d FM CF.t for Research and Ins ction of Alloys," of Accelerated Strauss Testmg," ASTM STP Ead4 rain in su pa-Transacnons, Am. Soc. bel Treatmg, Vol 18, 369,1963, pp. 235-239.

(9) Subtle effects due to vanations m copper sur.

1930, p 1126; also, " Report of Subcommit-tee IV on Methods of Corrosion Testmg, face areas, galsanic contact, condenser de- -,3,3,,g,,n,,,

,,c gm c, 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- , u ,, ,,,g lung des Redompotentials der Strausschen Lo - ' , To dais' eo dat (4) For details, see DeLong, W. B., "Testmg Multiple Specimens of Stamiess Steels m a sung mit Zusatz von Mettahschem Kupfer,'

Modified Boihng Nitnc Acid Test Appara- Corrosion Science, Vol 7,1967, pp. 501-511.

rus,* Sympossum on Evaluarson Tests for (10) Brown, M. H.," Behavior of Austenioc Stam-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.

1-12.

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

AISI 304 l

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

~

• - - wJ O(O,- M h M N %,"MM6MN,k3 3 ~c:imm eW a ___f _

s. ., *-

w--. _.,,i, m

( --- -- .__ . _ _ _

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 p g invesogated bs bending a seeet,

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

'b=

E N grad s of usin. css weeis .n h.sh thes ma. %e foun d Thew tsis ma, caatain stades of weels n add oon to show g ca ia '

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 b

I

, nons Recorr menJeJ % l

• [ { g. ~ g ~,

nc al Rencan. A rn l h1941 M4 LG4 L 116 ion of 10 "c mir's 1 7 sl5l= M4 . iga t fAISI liAL ll? Il?L Afsl 116 Il6L

1. M t see W arrea D (F 1 CF 4

,' b I

,d Es aurmn Test tar

'% u l' CF1 CF< f Kl C F I M C F il M ll' )l'l

' I M.L Steel ' A S T if 8,de: n f l k.

pp 45-5$

• Copper Cspeer Sulfate hE

• acce!erve the mterittan- F em suh Swifanc Acd y, g ,p gn .

istzed Justeninc wa.nien y , nc y , 7,y , 7,3 , , ,

Teu s i 0 m .n Soihng Teu i 4 % u 'O C i d Tesi a 4m 3 i,c , n ,, , %,, ,

'**"'3"' N# * * 's wiu ocai

'n bodie

te-wifuric Jud was first '

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 d

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 II'l CF ) CF4 It'L 321.34' m wra w ar de and

! in of the copper capper ' ' ' ' ' pe a se .a* lie C % rommm care.de aad s.sma est, see hharfuem. L C N1. An Esalu4non "*' "' " 32 ' " ' ' ' ' "

• C"*

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.

ed by Her5ie5 G ana r1uchungen zur Ernstel-

• • C3 ^"*'C""8I"""#'d**'"""'

"' " " " " d ' '" " ' " # " ' P r "'d ' " ' 5 ' 30* 3 ' O '# * '"d ' ' S ' ' ' O # 30 ^ ' na AC I C N . ' u h.

• """*"'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 i

'o Inter c aNar L}orro-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 i

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

EL 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'n canno. se wreceed 'setwe 4ese s,adei m. conica a i,x or , ,m a pha,e .n<a ,s ,

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 Da s l Y[

usi w s.ee D a Ead cr&a i sn  ! ,,. % :,

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

i st%Istel %ep Dual Ead Gera 11 ll D'i d l

[g ,,( j sisi it' vep Dual E ad Grea i l 14 Ddd  :

A '

sisi )i'l vec Dus E ad Ger a I & 11 Doch l F Aisi m some ..

T y

ACI CF 3 Yep Da Iwurd Fernie P*n D1 6h l a'e Ne a d t - s D%aes p x'

SCI ( F 9 Siep Dwai Iwlated Feroie Pws De laiemeadr% Dmacs t Yep Duo Iwurd F ernie Pws D%h laie oeadra s D icars I 4 ACI C F-lM i SCI C F eM Ster Duai Iwlated F ernte Pain Dit c h l a r c +ccad r*is D4sies J E*% .

• sereme a. 'sa.ms a cw sira uemuu r 5e tenied 'a t ac

• e*' s suifee voar i. 6 d te's ,.

x m,$

1,b.

h., *.6 are. a.

k ++ . gI g e d . +

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 Acceptable lich Structures Nonescepiahn s lish Siructures*

Grade Step. Dual. End Grain 1 Duch. End Grain 11 AISI 304 Dnch. End Grain il Alst 304L Sier. Dual. End Grain i Duch, laserdcadrnw Onches AClCF.h Step. Dual. Isolated Fernte Poots Deich. Interdendenic Dushcs ACI CF 3 Sier. Dual 1=ol.ned Ferrue Pooh

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

,y m% fa '

TABLE $ Use of Elch Sareciere Clasifkseiens from Tess the Osel6e Acid Elth Tess Meh 10 3 4 Nterte 3 % H drofluorie Ae64 "d"'**'I" Asseriable Eich Sirustures N

• Sirvi;iures

• '" 'P' '"["

Grade T reat ment A prece,*cd* Step. Dual. End Grain I and 11 Dach AlSa 3 6 Onch A preces.ed

• Step. Dual. End Grain I and 11 AISI 317 Dual. Dach As reces.ed Siep. End Grain i and il AISI 316L Siep. Dual End Grsin I and 11 Dach Senuaired Step. End Crain I and il Dual. Dach As-received

"'S'3 Step. Dual. End Grain I and 11 Dnch Senuiered

• 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 s must be laboratory. annealed in order to produca a baw hne specimen having a saep uructure The laborators.annea ed ~

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.

Acceptable Etch acceptable Each 2*- Grade Struc-Structures tures*

Alst 304 Siep. Dual. End Ditch Grain I and il AISI 304L Step. Dual End Dach Grain I and 11 Step. Dual. End Onch AISI 316 Grain I and 11 Step. Dual. End Ditch AISI 316L i Grain I and 11 8 Siep. Dual. End Dach AISI 317 i Grain I and 11 Step. Dual. End DHch l

" AISI 317L

• Grain I and 18 Alst 321 Siep. Dual. End Dnch '

Grain I and 11 '

Step. Dual. End Dnch AISI 347 Grain I and 11

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

i8

.NW 4

%Qf2ki as G W

6) H g

4 . &

Q .

i N

3

., A g

W 4[h A 262 i TABLE 7 Sues .f Tese Specimens n..

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

• ros,ekt sure or rod 7 L p to , in in diameter inct FoH diameter bv ) in tmin i .fz

• onacceceante E nh Strwiu es' r M", ty i

Desch End Guin 11 Over '4 in in diameter Cylandrical segment '.m d $,

Duch E nd (.rva 11 r hic s e= I .n i m a s , ..de , c?,j Dit c h e.

lescede n dr ts D.taes D.lch inredend t m D t s ss bv ) to ? .n ions

• g>j.

a ros,ekt t hre r sterp piarer

-1 N 4.-

>r *!ar tot 92 produrrr

? TY Lpm ..a m cm mci

Fu l 'hica nen bv e to I in e

}

..de B. ) ,n i min i ion e g' to % .%eme-3 % H.,drott.oric Acid O.er . in rMu t 6. to 7 in thsc h 9, e to I 4n .i de ev ) in s min ,

I Ts, bin g m... t . ,

g Nomau couede f.x" 5 v r uc t u re s* Up to l ' s m m diameter. Full rice t .a ..de

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

,, .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

'"' m, ~ ~,,<e ne he,d l

one .na.e sn.u he a orie,n. 5.aace or ine maierui c g ,,y e  !. -

nder test and it sha*l he on +e outside af the bead Couf #

4 coned Me* 2 dwphute ipcomen '

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

?' ' " ' "

_,,,,,,,,,,g,,,,,, NW 2::::"::: :he"':c::

m ,,, ,

3, - .-re~ re ~ ~~~-.~

l.<~...e..e_.,.n_ s -, D-- , - ~ n - },s q j . ei.ed s pe-c e ,... e, a n,,,,wr,

'r the H NO, H F 'cu T ha reg., ce 3r 31tJt b .M 'me H Ns), H F .gy n

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

• d . a he corrown are >( en e wage , ce * '*** #

Iq g i

-n 4. c: %, 'Q / 't 5 5 k,L

.(.,.

.o j 'hEh

, . ry. . < . s.,

'l .

h; 'c$

s. . j.

.w.

.c . ,

, \> 4 ~

'x.. .

..'Y c d

, e t

,. .k 6a ,s - -

j e^ -5:

. 'G,b gd '~ .

-G . ,; ,;, -

t ,

.L

s. . ( '

3

" @g T.

I.S ' 'nT, c.

- 3 ,

,-r .e - -

- i, .

L.v i

, , a.

s a

m.g-7%

w.

s ., s t,,? J 6 , 6 , ), x w. .

v

, i n ;.e a e,. m. .r, x9 - ,  ; x y. . ,

h. my; t

,1c ,

T['

s,e , s. r.e .r e , , ... . . . s, e ,. . .e e . , r. ... .

W 's . .h k .

1 '. .l d.. . . .. ,r .. .r ...

r ,

b.

g,.... ,

I

• 19

J'..Iw

-r w .; . ...:,,..-

g; 4 -c + . .

. m .. . _.

m .7 -- - .-

- -- -- - ' D 2:'.(5 .

l

._ _. ~ _ _ _ _ _ . - - _ . ._ .. . - _

~

" ' ~' ~ '

, .',-  % 9; '%.:. Wor" *

%, ~ * [ ** 'E ~-

'-* y*Q  ;  : . , . ,

~

t h Sh' 9styg .

.s (h}h A 262

. p. -

.  % . y * .y y

~

• i y~ k ,A ',

• i .

e l .

. s., . . . . .,

, , ' f - .

s .' - '

g*

s y -

s. 4) * 'M c It p 4* \

4 g-  ; .. -

r ..

1. 'n .

, -  : / R

'4,.

i

s. .1 .

. :r V . ,, . .ep.. . .'v!

77

.g .

. g. , .

o -

,,f -

- S -

a e

t- .

.e

.1,. ;j / .

l MG. 2 Deal Structure (150 s I (Some d6sches es green beende#6es la add 6sion se steps, bee me ese grme completely nc. 4 Isolased I l _ sorrounded). f l

r I e' '%

. a ge 1

\  ; , \ %N .-

w -

s

; 'l

<, 1.

,t t..o..,.

b .

'.'* , 4 .' s f i 3 g[Of -

1. g.: i3-e , ..

. ., 4 - ,

.m  :-

j'j s r .

~

r.'

. ~S E $ :L '

nc. s se

,' T . . ..

nc. 3 naen serwi-e isoo ei come --e gro6ms e.-rie ei> -reended b3 d ne. . .

l 20 Yh. h,i.

l

.. x ... , w - '-

l&&hk.

=- ,

us

..ps x.e . ... .-

= i*.

mt -==..-

.ms3p_

w_ __ _ .

45h A 262 I

Y ~ .,

i, -

4 *

{f -%

. . e g

.- s. 1

E-

.K / * ...

.,o

g;,

p: . % .J g .f%d.9,'.et p '. i .

w.  % J

! Q,

'4

?). %. 3 . /* ' 'p

\  : i G. Yn . .n. . s. ,

T .

'? - . .

, e . . ..

1

' - l., ,)g

~,.

f..

s

, y ;&.

bos no e.e g.... compg..,,y F1G. 4 w i Isoleted Femae Poets t250= ) 40hened in castents sad = elds. Steps between easte.ere m art a s and femse peoJu.

[ . h' O

g .

f .

9 M* I

. ~ _ ,

)*

.g

~ .

e f

1 u

I I

V 4 * *

,r- ,

(

4 f

• 3

\

%e

• 4 d

j

1. 28

s. I gm ;. \

. g>r '; .

al

,,<.,.............o...s.,......-.d.......s......s.........c,.d....._,. . . -

fe.

3

• ,e ; y o

'y c-1

@y'M h 2 6 Y F M h / S9 '(*r f. # T @ N T W F

• N ? + ? ' " " ' ~

l __ . _ . _ , _ . - - - _.

4 i

M' W i.

l (h A 262 l i

l

• .ts, e .

I y_. . ,

t , ,

t -

a ,, A..

.- i r,# g ,,

' e  ;

s. . .

• • s .

s 6 I- o.4

, s .

.a.

n. * ~$ '& . r' /o2

• e, -  !

i 6 .. . v.

,*<-o'. . '. . a I *

t. .2 . , . .

a l

949 ,@ .% o.N . < . ' -

l' j i

[. o Y [,r J'o, t.g l .

4 ' .gf . ' t Jp .

~

To d#erenuate between the typ'es'~of pts.use a magnificaison of 500 = and focus in the plane whsh now appear completely black are end grain pts.

4 FIG. 6 End Greis Pteting I(500m)(A few deep end greis pies (see 1 le flgeren and shanew each pies (21 1

b

. . . . + - ,*.....~.

, -i ... -

. m- . .: /.- 4a.-,e...\ - .

V --

~~'

' v..?.f+, O.'

Y:" E.;*, E:.$.] t

~ ~

k.-

.jt

. O m, q . %-~.

q. ;f

'/ J'y, h.-.w?/j

". .*/p;,.%.>. l."

' /'fll.;fj i r-q..  ;. .

" g'.t' ;

,~ &g' .

i

/- .; -  :'t a- ,k. -

4 *, $ p,,,:,' -Je g ,f/ ... . at j g, . . . W l.t* . ? ; . o.3 o.< _

• Q, .t .

i . . \., z--- e-

?

.e g- *e Y' ) '

, . . l - -

-r- I f '.'

+s

, 2~~ f,

%:. J . ..I,'. %;g,, ..

s.

- s%' .+..M

-'.[ ,'

' ' ~ '

• f- .. e ' 9 ; ,,. ,

w w :S

. ' - . ~ - 4. 2

~ .

],

. N- ~ .' g  %. . >

. _ m+ . . > .s1,f.

f- ,

e-u g The or a greater concentranon of end grain pis at 500 = (using standard etching conditions)indgates th must be tested when screemng is for nitric acid test.

FIG. 7 End Greis Pteting II (500 m p.

l 22 f

. I

. , _ ..r..

- =: Pnhd. M. ,g

s. - ,

p.1.e..- '.; ,+.

A, .,,

2 5-

.9:* .-

w.

NT

- f.is

~

lI l

$tl j za _

_ _. _ ., __._..-___ .-__-~_ _ _____ ._______ _ __-

QW. gg - %~"fggggg" g I M:

.o ...? + ' .- d:

4*ww mM$f.:.v%". c-141.3

^

x m - q3Q. 4w tea ^p, ., Q ~ .= . 'Ap*~33 1 - .g_. . --

(h A 262

. .s n .% <

b 'N ' l "N..

-( Wir e to fosten tu bing ,

• • f Allinn condenser 4

4 belDS, joinf **

W O O

);I / y 1

g L.* 5& nn c.

}/h Cooling .oter y ' , .s

,~o 1 later Erlenmeyer

.'s.F s 4

. x, '

?# .I'

1. flo t h wif n loin t ,

Ugg g elic o n es f.

Stopcock greste

< >'  ?

s .

i , Q .

G'*"*'"*' -

<S s o,i,n g e n. . . ,a _n etched surface The p..,

'*' '2g '" * *

}

2-'A low each pets (2)). Ja- i j

' 9Jl j

.y- -J ~ .,

l s

~g':

-3 N 2 - --

P. ,

51G. 8 Apperseus foe Ferrw 5eJfase.5.iruru 4cui Test.

4

",e o .

hlql h '

i +f. *Y

.- - 40 m m- . L20.6 mm ) $

I

( tr y J" ~* ~ 7 li, 31 mm

$ k.s.8 mm TUSING ii ii 4 N

63 5 mm asom D  : ' - '

, E.

p.

- f ^ l 76 mm P

'/\.;

. 4 6mm

! I i 1000 mt ..

I ','3g ,\'[- wiOE MOUTH i,- vc y_ . u__.- I - U FRLENME YE R

_ g CONDENSER FLASK y }

FLASK wiTH CONDENSER 4 ' .'

E . NOTE CONCENSER MADE IN PLACE k #~,

d

. OF PYREX OR EOulV- I. n 4 g ALENT ME AT.EESISTING

-; glass E.

j I

e s i n. i s, ,,,,c ,,, nc. , n..a ..a c 4e..er te. Neerw a c.4 Teu.

he... 3, W.

1 . . 4-n 23 7 -

e A . ' , ;-

-r . p,, j ,

....n e - ~ '= J-'- -

2 ~ u v- e a} , cz .< gr.3. n .=._: .~

[' V 2,l: .

• q; ($}h A 262 ,

i Glass Condenser y j

Tube (10 mm.)

___ - Water Trap Polyethylene Sheet (6 mil)

/h f!h j

j

~ {"(

l t

l l- Pipe (Polyvinyl Chloride)

1-114 in. ID x 3/16 in. Wall

{ { x 12 in. Long) i t- TFE-Fluorocarbon Cord l l s

!- Specimen Helder (Made from 3h:=:x TFE Fluorocarbon Tubing or l

t

,?. , { Polyvinyl Chloride Socket- j

{Q  : type Cap) l @pp

3  : A W! [

l  :

3

1 NOTE: Cylinder Must be \ ottom Joint Consists of B 3

} '.5-Clamped or Otherwise Fillet-Welded PVC Disk or Supported in Water Bath , g Solvent-Welded PVC Socket- -

Type Cap j-j e

FIG.10 Appersees for Nrrte.Hydroneene Acid Test. -

i a . ~i n h

4

M4nt i  ; av si i '

• i

' ii 9

v4 I

l a E E i

_~ M .

nG.12 Pas s

24 p fh.'a f f f *~ ~

"Wl}'#Mgj&$"

TE ;..

I .+ bi efg p m p- 4

' <Ayrwg;46tch

• yfm gd# .

"=, ..=

Q{%g.

Y 5 n: w&N-?"?',$

O f *~ *z j .. a w'

q

' _ i. _ ,., _. __ _.

f ~

• .. ~;.2'?

.. : +.. 5; y , .g '. [b ' ' ( *

. %: . . I .N

%*Wf A

..y  ? -- y -- --

'3

' :- - ~

.___._C_- wQ - - --

g_ ,:i:= ' ?

% . * ' - $?.* & .7..w" a m . . 6 ?-

~

_ _ . _ _ . .- _ . 4, . .a-en _,

":?$'

1 4h[h A 262 Irap

• t  !

't Stopper 1 Tl ' '

iyl Chieride)

I J x 3/16 iri. Wall i

0 l , .

i i I

acorbon Cord s.- .  ; -

y i

Ider Odade from nc. :: A seen c pu s.u. ser.nc Am

orbon Tubing or

'oride Socket-e.) .

, insists of

," ' '.1 g .;

/C Disk or

{ , , t . .

',,,(,,.;4.pp^

j .

PVC Socket- * -

J

- .i ,

lj "ut. y i

[4 l

?. . ,

'k ja-c W Qda, 'M,h i i  !, J 1 4 r A .. Are

< i  ; 4 vi *Q '. C , s%W0 .

i a ,  ;, -

3 ~ 15 $ i &

.6 i '

s wJr# mg _ . i c  ;

RC. IJ Peneng Tess 5 penmen-W= ef the Bees Aree. (20m magneticades befor, reprod.csseep. [ ,, .

. 3 2s

. pg%Q:,.T f?hhk h$$$hNSW5[ W s M W =

(h}h 4 262 I

g )

m . }

l a ,

g .

e' 3 f* g M i g) $

"p ,

T' .l fr F1G.13 Failing Year Specimen. (Nose ibe many intergrenelar nuores. Ben area se 20 m magadication before ric. 34 Deshtf repredsettoe.)

b Thr Amerecae 5 of 4r se s o ,

i e Thns vandard . \ '

-- ) . wars and { not

• s

' for ad.inoe..nal stor

• )- at e

• ret ** t of

a fair heurang ses 1910.1 . nera a el

\ -v

• AST.st B.ard of. '

.d s.

, . + ' i

- 4 l

r yfr ,

! i r }

5 $7 3

UMXW 9 - - _ _ _ _ - _ _ . - - - - . _-._ - _ - ,

..,a- -( ' Mh , _

YW* ~? fe

'3U_TELwM , ,. ,

^

6 N'

4. . *Yf a h .

e".*

• • ] ., .

l ,

Ik kb A 262 ',

• [5[*

, n-4, e

_ 5- ,Q.

i

-y $.

• g 4

\

• tes e- 4 .

5

=

$ N, '

s -

F "

{

(

u .,

I g '.g [.

t Wp% ,;T } Pl$y K _  ?  ?

'l w g

nz.

, -t Ag - i r .h

.e, e r ,w .

~ .

sv. x

" 1 , , se y

. ~. '

f {'

6 a

k.- '

n

• ~

n

.L *

, messhoe before FlG. 14 Desbefel Test R le. the traces ofintergrenelst Asseres and "ers e. peer' surface. Bent are. et 20 m magnefkstion before reprodection.) '

~'~

~ ~

, 4 The Amorecen Socortsfor Testung and Mattreals takrs no possteon erspectent the valsdsts of ans partor rechts asserved #

nn conarctson estk any stem menteoned sn th<s standard Users of thss standard are espressly advused that determsnarson s '

ofthe vassdary of ans such patent erqMts. and the ensk ofonferngement of such rrghts. Ls enttrely their Own responsnbtlEty '

l Tha standard as subject to revuson at any Isme by the responsuble technocal commotter and must be reverwed evers five

• • ers and of not revurd. ruhre reapproved or ankdrawn i

!** ad.lotovoul standa-ds and sk<uld be addretted to ASTM HroJguartersYour comments are sneurd erther for y revuson of this stand .

Your comments edl recerse careful cons >derasson an a mers,ng of she responsable erkeneal commettre whach vou mar attend if you feel s' ear your comments have not erressed e farr keurong you should make sour vores known to the 4STM Commotter on Starards r

19tt)I loin Mace St . Photadr ophra Pa \ .a'.

l whn k well schedule a furskre krareng regardeng your commress Farlong at sfactron three you may appeal to the '

I 45T64 BourJ of Dovernors *

{ E l

6 t

r

". /.

l l

'}* ,

if d.

L it

• c

,,, f i k.

y,s , ,e 27 1

F4 ]

, .a

-