330 643 9076 P.

02
ASTM £353 ~3 II D?5~510 052SA4b ~72 II

Designation: I! 353 - 93
Repl _ AMERICAN

114111I
,91'
SOCIETY FOI'I tesTING
Race III Phl"",.lp"'"
AND MA1'eFlIAL5
Pa 1910:1
tile AllIIUIII 800_ 0'1 AStM 5/tllllald.. C~WlIOI!t AStM
If n.ll;"ted in !he c..rent combined Index. will a~e.t ;n Iha nell adft:Otl,

Standard Test Methods for

Chemical Analysis of Stainless, Heat-Resisting, Maraging,
and Other Similar Chromium-Nickel-IronAlloys'
Thil ,..adll'll il WII" under Ihc rwd dGianlltion E JS3; tbe number jmmcdilltcl~ following the desiJllllIiOll inCllmes Ibe year of
oriainal adoption or. in the cue of revision. \he year of last revision. A number in plltI!lItheJes ;ndieatrs Ilia )'~ of bli reapprgvaJ.
wpcncripl cpsIIoa (t) ind1ct.tes an e4ilOria' cJI.. &inee \he last revillon or =JIPfOval. "

1. Scope 5=iotll
Copper by Ihe SuiCide Pn!ciplt.:ltion-tleeuodcpolition Gnlvimetric:
J.J These 1eS\ methods2 cover the chemical analysis of Method(0.01\0 5.00"). . . . . .. . .. . .. . , .. .. . .. . . . . . . . . . .. .. . 82
Lead by the 10n-£aellallac-AlOtIIic AbIorption Mcillod (0.00 I 10
stainless, heat-resisting. maragins. and other similar c.hro-
O.SO ") . . . . . . . . . . . . . . .. . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . 12'
mium-nickel-iron alloys having chemical compositions "'anaancse by the PcriGdale Photomelric MMod (0.01 10 5.00 9&) ... 8
within the foUowing limits: MoIybdellllm by lIIe Ion .Eitdl8IIJC-1-HydroayquinoJine Cnlvimarie

Elemenl Concenll8UOnRange, MClltOCl ,... ...... . .. . .,.. ...

. 242
Molybdenum by the Photometric Metllod (0.0110 1.50 9&). . . . . . .... 190
Alumlnllm 0.002 to $.50 " Nickel by file Dintet/lylalyOllime Gravimetric Me1hDd (0./1048.0 ")
, 172
BorDII 0.00 I 10 0.20 PIIOSPllorus by Ihe AIIWIAICltic MetbocHO.02 10 0.1' ") ... . . .. 164
Orban 0.01 10 1.50 PholC)boM by Ihe Molybdenum Slue Pbol'Omelric Mflhocl (0.002 JO
Chromium e.G1 1035.00 0.35S). .... . ... . ... ... . .. . .... .... .. . . ... .... 18
Coball e.G, '0 IS.OO Silicon by lIIe GraVimetric Mablld (O.OS to 4.00 '1» ., '" 46 .
Columbium INiobillm) 0.01 to 4.00 Sulr".. by theCn,imetnc Method _. . fit-'
Copper 0.01 (0 S.OO Sulfllt by Ibe Combultion-Iodarc Ti!l8tioo Melhod (0.005 to 0.5 ,,) 31
Lead 0.001 (0 O.SO Sulfur by 1M ChrollJll\Oil1lphic Gravimetric Method. . . . . . . . . . . . . ". . 1&
MllnpnclllC 0.01 to 20.00 Tin by the Salven~ Eall8ctioD-Atomic Ablorption M..!locI (0.002 tCl
MoJybdenllm 0.01 ro 7.00 0.10 sr.).. ., . . . .. . .. . . . . . . , . . . . , . . . . . .. . . . . . . . . . . . . , . . . . . . 110
Nickel 0.0 I to 48.00 Tin 11)'the SIoIIideoJodol\1Clric Tittation Method (0.0 I 10 O.OS \is) . . . . . 90
Nllrolell 0.00110 0.50 Tilallium. Total, by tile DintipyT)'lmctbane $p=lropJIOIOllleuic
Phosphorus 0.002 to 0,1' Melhod (0.01 10 0.3S ,,).. .. . .. .. . .. .. .. . .. . . . . .. . .. . . . . . , 23 I
Selenium 0.01 to O.SO Vallldi"m b)' \be AIOlIIieA~~on " Melbod (0.110610 0.1' 1'5) 221
Silicon 0.0 t to 4.00
Sulfur 0.002 to O.SO I J Test methods for the determination of several cle-
Tanlaillm 0.0 I 10 0.'0 ments not included in this standard can be found in Test
Tin 0.00 I 10 O.OS Methods E 30 and Test Methods E 1019.
Tilanium 0.01 10 4.50
Tun[lSlen 0.0 I 10 4.50 1.4 Some of the concentration nmges given in 1.1 are toO
Vanad,uDI 0.005 10 1.00 broad to be cov~r\'4 by a single test method and therefore
Zirconium 0.00 110 0.20 this standard contains multiple teSt methods for lome
1.2 The test methods in this standard are contained in the elements. The user must select the proper test method by
sections indicated below: matching the infonnatioQ given in the Scope and [nter(er-
Sections enee sections of each method with the composition of the
Aluminum. TfIt8l. by lite 8-Quin<.llinol Olllvillletrlc Mcl!loG (0.20 10
alloy to be !\Dalyzed,
1.00 ,,) 119 1.5 The values stated in SI unirs arc to be regarded as
Aluminum. Total. by the 8~uinolinol Pltntomeuic Method (0.003 to standard. In some cases. excep\ions allowed in Practice
0.20%).,... ,.. ' . . ... . 11
C.:ttbon, TOIaI. by \lie Combu&lion- TItcmsaJ CoftdllelivilY Method. . 1#1 E 380 are also used.
ClUbon, TOIIILb)/ Ihe Combusrton Gravimetric Mflltod (0.0$ 10 1.6 This standard does not purport to address all of the
1.50 'Ii) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . . . . . . . . . safelY problenu. if any. associated wilh ils use. II ;s the
'8
Cllromium by the Atomic Ablolplion Melhod ' (0.006 to 1-00 ~) . . . .. 202
respolUibllil}lof Ihe user of this standard to eSlablish appro-
Chromium by mo I'ero"Ydisvlllice Oxldadoll-Titrallon MelllOCl10.10
10 3S.oo ") ... , . .. .. , . . ... ... .... .. , . .... . 212 priale safety Qnd health practices and determine lire applica-
Chromium b)I the Peroa)'llilu.tatc.Oxidalioll l1Uimctric Mclhod . . . . . Jb bility of regulatory limitations prior to we. Specific hazards
ColJaIl b)/ the 1on-~haa._PolClI!iomctrie TIIlaUODMCIhod (2 \0 statemenrs are given in Section 7 and in special "Warning"
1$."). ., . . . . . , . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . .. . . . . . . . . . 53
Coball by the Nitroso-lt.SaU PhOIOmetric Mclhod (0.11110 5.0 %) . . . . paragraphs throughout these test methods.
COPIICf' b)/ lhe N~PI'oille PhoiOGleU'ic: Method (0.0110 5.00) \is) . . . 109
"

2_ Refereaced DocumentJ
I Thac ICIt methods .ue u.nder 1/Ie jllNditlion at ASTM Commitlee E.-Ion
Analytical CbemUIIy far Meta4, Om, and Rc1a1c4 Materials and ue tile diftCt 2.1 ASTM Sumdatds;
mpgllilllililY ofSubc:Gmmlnee EO 1.0 I Oil /1'1111.SreeJ. md Fermalloys. D 1193 Specification for R.eagell1 Wa\er'
CurreBI oditiOIl aPOro~ July IS, 1993. Pvbliahecl Septentber 1993. Orisin~ly
E 29 Practice for Using SigrUficant Digits in Test Data \0
publisbed
j 115 E
3'3 -
11Iac tal motllOlSc repnscllt
fi8 T. 4Jt
",visions
previo," ediricm . 3S3
0( IIII:IlIod! eavercll lIy ASTM
- 89.
.Determine CODfonnancc with Specitlcations4
Methods E 30 and E 31 ...hicJla i.. lhi. plibliclllion.
2. DiIiCClRWlUc:d Aflril 25. 198&. 11$ replacement 3ppc&n lIS pari af ASTM
Merhod E 1019. found in A,,1f/IQ18ou1c qf .4STM SlIl1lt/tWI. VOl OJ.OS. ~c Diseolllinuc:d April 19, 1988.
IA Disco,ulnued May 30. 1980. J AIIlfIlDl BtJIj/c (If /CSTM SlmulJJ,tb. VB! 11.01.
4 ANllltli B()(J/( of /CSTM Sl."d~. Vol 14.02.

ASTM £353
E 30 Teat Methods for Chmical Analysis of Steel. Cast
Iron, OpeD Hearth Iron. and Wrousht Itoz&'
E 50 Practices tor Apparatus. Reagents. and Safety Pre.
cautioD for Chemical Analysis of Meta/ss
E S9 Practice for Sampling Steel and Iron for Detennjna.
tion of CbcmicaI Compositions
£ 60 Practice for Photometric ud Spectrophotometric
Methods for ChemicaI Analysis of Metals'
E 113 Practice for Conducting In18liaboratory Studies of
Methods for Chemical Analysis of Metalss
E 350 Test Methods ror Chemica] Ana1ysis of Carbon
Steel, Low-ADoy Steel, Silicon ElectricaJ SteeJ, Ingot
Iron. and Wrought [ron'
E 35 J Test Methods ror Chemical Analysis of Cast tron-
AllTypes'
E 352 Test Methods for Chemical AnaJysis of Tool Steels
and Other Similar Medium- and High-Alloy Steels'
E 354 Test Methods for Cbemic:aJ Analysis of High.
TemperatUte, Electrical, Magnetic and Other Similar
Iron. Nickel. and Cobalt AlloysS
E 380 Practice for Use of the International System of
Units (51) (the Modernized Metric System)4
E 882 Guide tor Accountability and Quality Control in
the Chemical Analysis Laboratory'
E 1019 Test Methods for Determination of Carbon.
Sulfur, Nitrogen, Oxygen, and Hydrogen in Steel and in
Iron, Njckcl, and Cobalt Alloys'
D 1024 Guide for Cbemical AnalySis of Metals and Metal
Bearing Ores by flame Atomic Absorption Spectropho-
tometry'
E 1097 Guide (or Direct Current Pwma Emission Spec.
trometry Analysis'
2.2 Other Document:
ISO 5725 Precision of Test Methods-Determjnation of'
Repeatability and ReproducibiJi1y for Inter-Laboratory
Tens'
3. Sicl1in~ce add Use
3.1 These test metbodt forlhc d1cmical analysis cfmetals
and ano)'!! are primarily intended as referee methods to test
such materials ror compliance with compositional specifica.
tions, panicularly those under the jurisdiction of ASTM
Commiuee A I on Steel, Stainless Steel, and Related Alloys.
It is assumed that all who use these! test methods will be
trained analysts capable of penonnia&. common laboratory
procedures $kil1fuJly and safely. Jt is expected that work: will
be performed in a properly equipped laboratory under
appropriate quality control practices such as those described
in Guide E 882.
4. ApparahlS, RealentJ, and Iastrumental Practices
4.1 A,pparazus-Speclali%ed ~paratus req~iremel\ts are
listed in the "Apparatus" Section in each method. In some
cases ~r~nec may be m.cc to Practices E SO.
4.2 RetAkenls:
4.2.1 Purity 0/ Reagents-Unless otherwise indicated. all
BpO/r. f1/ tfSTM SWtdtI1d.1. Vol 03.05.
'''""1141
. JJ_III ASTN SIIZIfIigrrh. Vol 03.06.
.. """rIIII
A¥8iIable IhIm Americall NulOIIaI SWlIWdIIJIst!tUIe. II West 41nd Str>eU.
13th 1'1oor. New York, NY 10035.
330 643 9076 P.03
'3 II D7S~5LO DS256~? &D' II
(rI}t E 353
reqents used in these test methods sbaU conform to the
"Reagent Grade" Specifications DCthe American Chemical
Society.8 Other chemicak may be used, provided it is tirst
ascertained. that they are ofsutrJciently lUsh purity to permit
their use without adversely affecting the expected perfor.
mance of the determination. as indicated ia tbe section on
"Precision and Bias."
4.2.2 PuritjJ of Water-Unless otherwise indicated, refer-
ences to water 5ha11 be uudcrstood to mean reagelu water 8i
de.fiDed.by Type U ofSpecifiwion.D 1191.
4.3 Photometric Practice-Photometric prescn'bed in
these test methods shall oonfottU to Practice E 60.
S. Sampling
S.l For procedures for sampling the material. reference
sball be made to Practice E 59.
6. Interlaboratory Studies and Rounding Qd~ulated Values
6.1 These test methods have been evaluated usins Practice
E 173 or ISO 5725.
6.2 Calculated values shall be rouDded to the desired
number of places as directed in 3.4 to 3.6 of Practice E 29.
7. Hazara
7.1 For precaudons \0 be observed in the we of cenain
reagents and eq,uipment in these methods, refer to Practices
ESO.
MANGANESE BY THE META PERIODATE
PHOTOMETRIC MlnlOD
8. Scope
8.1 Tbis method covers the determination of manpnese
in concentrations from 0.0\ to 5.00 %.
9. Summary of Method
9.1 Manganous ions arc oxidized to pennanganate ions
by treatment with periodate. TUDgsten when present at
concentrations sreater than 0.5 % is kept in solution with
phosphoric acid. Solutions of the samples are fumed with
pcrchloric acid so that the effect of pcriodate is limited to the
oxidation of manganese. Photometric measurement is rpade
at approximately S45 11m.
10. Concentration Range
10.1 The recommendedconcenuauon raDge is 0.15 to 0.8
m.g of m8nlaftC$C per 50 mL of solution, using a J-cm cell
(see Note [) and a spectrophotometer with a band wieith of
10 nm or les.s.
Nor! I-This m~ocI hu been writCtl\ for ceUs h4viJif II I~ \iib1
path and a "nllTow-band" iAs1n1ment. The com::cntntion ral\le de.
(lelICUupon band width and spectral region used as weU as cell o~caI
IIlIth Icnath. Cdls bavins otbw dimensions may be used. provilkd.
l!U.ita.bIeadjustmenlS can be made in the amounts of sample land
rellgllnts u5ed.
I "R8apII1 ClcmicaIa. Ameticasl Chemical SocieI.)' SI*iIiCCItilm.." Am.
Chemical Soc., Wuhilllloll. DC. For i_ on lite ImiDa of Reaacau 1101
Ii_ by the Amcriull CIIemIcaI$ocIc1y.sa: "R_III CMalitals r.mI ~..
b) 10Sc»b RClliD.:C. Vu NCIIUUd.Co.. IIIc,. New York, NY. aad !he "Vni\Cd
SuHS PbrmlS'l)pCia," UDiIIJCISlaW PII~qpciaI CoIMtDLion.Roekvine, MD
;roSS2.
2
 330 643 9076 P.04
ASTft E353 ~3 II 075'510 Dg~5&~6 TQS II

41 E 353
11. Stability of Color
11.1 Th= c:oIor is stahle for at leut 24 b.
12. Interferences
12.J Perchloric acid treatme.lu, which is used in the
procedure. yields solutions which can be hiahly colored due
to the presence or Cr (VI) ions. Although these ions and
other colored ioes in the sample solution undelJo no funher
changc in color quality Upon treatment with metaperiodate
ion. the fof)owing precaulioos must be observed when tihel
photometers are usecl: Select a (alter with maximum uans.
minance bc1ween 545 and .565 nm. The filter must transmit
not more than S % of its maximum al: a wavelength shaner
tban 530 11m.Tbe band width of the filter should be less tban
30 om when measurecl at 50 % of its mwmum transmit.
ance. Similar restric:tionsapply with respec:l to the wave-
length region employed when other "wide-band" instru-
menu arc used.
12.2 The spectral transmittance C\U'YCof penrnlnpnatc
ions exlu'hiu two useful minima, one at approximately 526
nm, and the other at 54S nm. The latter is recommended
when a "narrow.band" spectrophotometer is used.
12.3 Tunssten. when present in amounu of more than
O.S % interferes by prOducing a turbiditY in the final solu-
tion. A special procedure is provided (or use witb amples
containing mOre than O.S % tungsten wbic:h eliminates the
problem by preventing the precipitatioD of the tunp1en.
13. Reagents
14.3 Color Development-Add 10 mL of KI04 solution,
and heat the solutions at not less than 9crC for 20 to 30 min
(Note 2). COol, dilute to volume with pretreated water, IUtd
mix.
NOTE 2-lmmcnina tbe 0uIi.& in a bl.Jilins water ba1h iIi a pufcm:d
muos or hutins them for th~ apecificd period to enSUre eomplck c:olor
development.
14.4 Pholometry:
14.4.1 Mulfiple-CellPhtJlonrerer-Measurethe cell cor-
rection using the Reference Solution (14.2) in absorprion
cellswith a l,clI1fisht pat.hand usiDga fight band centered at
aJ)ptoximately 545 am, Usinl the test cell, take the photo-
metric: readings of the <:alibration solutions versus the
Reference Solution (J4.2).
14.4.2 Single-C,II Photomeler-Tnmsfer a suitable por-
tion of the Reference Solution (14.2) to an absorption cdl
with a 1-cm lipt patb and adjust the photometer to the
iniriaJ settiJ1&wing a light band centered at approximately
545 12m.WbiJemaintainioa this adjustment. take rhe photo-
metric readinp of the calibration solutions.
14.5 CalibratiOl1 Curve-Plot the net photometric read-
ings of the calibration solutioDS aaainst miJiigrams of man...
Banese per SO mL of solution.
15. Procedure
15.1 Test Solution- Select.and weigh a sample in accor~
dance with the following:
t'olUllnCl! III

13.1 Manganese, Slandtml Solution (1 mL = 0.032 mg Samllle 5ampIe Dihllion. o4liqllOI

Manpncsc. \Vei"'". WeiJJIt,m. mt. Volume. mL
Mn)-- Transfer the equivalent of 0.4000 8 of assayed, high- "
purity manganese (purity: 99.99 minimum), to a SOO-mL 0.01 10O.S 0.80 O.S 100 20
" mL or HNO, by heating.
volumetric flask and dissolve in 20 o.4S 10 1.0 0.3~ 0.3 100 20
Cool, dilute to volume. and mix. Using a pipet, transfer 20 0.1iS10 2.0 0.80 O.S 500 20
J.9S 10 S.O 0.80 O.S 500 10
mL to a S()()..mLvolumeuic RISk,di]ute to volume, and mix.
13.2 Nitric.Phosphoric Acid Mixtul't-Cautiously, while Transfer it to a 300-mL Erlenmeyer flask.
stimnc. add 100 mL of HN03 and 400 mL ofHJPO. to 400 15.1.1.1 To di$iolve samples that do Dot require HF. add
mL of wa.ter.Cool, dilute to I L, and mix. Prepare frc:sha.s 8 to 10 mL of HCI (I + 1). and heal Add HNOJ as needed
needed. to hasten dissolution, and then add 3 Co 4 mL in excC$S.
13.3 PottUsium MetQperiodate So/utiOl1(7.S g,lL)-Dis- When dissolution is complete.cool, then add !O mt of
solve 7.S g of potauium metapcriaclate (KI04) in 200 mL of IiCIO.; evaporate to fumes to oxidize chromium, ifprcscnt,
hot HNO, (1 + I), add 400 mL ofH3PO.. cool, dilute to I L, and to expel HO. Continue fuming until salu begin \0
and mix. separate. Cool, add 50 mL ofwatet, and digest if necessary to
13.4 WaleT, Pretreated with Metaperiotiate-Add 20 mL dissolve tbe salts. Cool and transfer the solution 'to either a
of KJO. solution lo J L of water, mix, heat at not less than 100- or SOO-mlvolumetric flask as ind.icated in 5.1. Proceed
90'C for ZO to 30 min. and cool. Use this water to dilute to I.'S.L3.
solutions to volume that have been trcated with KI04 IS. 1.1.2 For samples whose dissolution is hastened by
solution to olCidize lDanpnese, and thus avoid reduction of HF, add 8 to 10 mL ofHC (1 + J), aDd heal Add HNOJ
permBJlgal1ate ions by any reducilll agents in the untreated and a few drops ot Hf' as n=dcd to hasten dissolution, and
water. Cautiol\-Avoid the use of rhis water for other then add 3 to 4 mL ofHNO]. When dissolution is complete,
purposes. cool, theft add 10 mL of HClO.. evaporate to fumes to
] 4.1 Prc}NIration of Calibration Curve oxidize chromium. if present, and to expel HCl. ConrinCAe
fUming until salts begiD to scpara~ Cool, add 50 mL 0(
14.1 Calibra'lon SolWions-Using pipets, trallsfer S, 10, water, digest jf nccessat)' to dissolve the salts, cool, and
15,20,and 25 mL ofmanpnese standard solution (I roL = transfer Lhesolution to either a 100- or SOO-mLvolumetric
0.032 mB Mn) to SO-mL borosilicate glass volumetric flasks, flask as indicated in IS.1. Proceed to IS.I.3.
and if necessAry, dilute to approximate)y 2S ml. Proceed as 15.1.2 For $ampl6s Containing More ThIJfI0.5 % Tung-
directed in J4.3. sten:
/4.2 ~t:feren~ SC/Ulicn- Transfer approximately 25 mL JS.1.2.1 1'0 dissolve samples tbat do not rcquiIe HF. add
of water to a SO-mL borosilicate Blass volumetric flask. 8 to 10mL o(HJI'O.. 10mL ofHClO., S to 6 mL ofH250.,
Proceed liSdirected in 14.3. and ,}to 4 mL orHN~. Heat moderately until the sample is
3

cop,npt by Ule Am.erican Sociely or Te3I.ingk hteriws

Fri Sep 18 13:47:32 1998
 330 643 9076 P.05

AST" E353 '3 II D75~S1D D52S34Q bB1..

~msE 353
decomposed, and then beat to copious white fumes for 10to C sample wei&ht. I, reprcscnted
. in SO mL of the final test
12 min Or until the chromium is oxidized and the HCI is "" solution.
expelled, but avoid hcauna to fumes of SOJ. Coo~ add 50 17. Precision ItI1dBias
mL of water, and dige&t,if necessary, to dissolve the saJts.
TtaJW'erthe lolution to either a 100- or SQO..mLvoJumetric 17.1 Precision-Nine laboratories cooperated in testing
flask as directed in J5.I. Proceed to 15.1.3. \his method and obtained the data summarized in Table 1.
15.1.2.2 For samples whose dissolUtion is hastened by 17.2 Bias-No infonnation on the accuracy of this
mothod is known. The accuracy of this method may be
Hf":Add 8 to 10 ml ofH3PO., 10 mL ofHClO., 5 to ti mL judged by comparine accepted reference values with the
of HzSO., 3 to 4 mL of HNO), and a few drops of HF. Heat
modentely until the sample is decomposed, and then heat to corrcBPOnding ari\hmcdc average obtained by inter-
laboratory testing. .
copious white fumes for 10 to 12 milaor until the chromium
is oxidi7.Cdand the HCI is expeDed, but avoid heating to
fumes or S03' Cool, add SOmL of water, digest, if necessary, TABLe 1 &taIlIUCIII"roI'l\'llUon-Manpn... by tM
Metllpellodl" Photamelric Method
to dissolve Chesalts, cool, and transfer the solution to a 100.
or SOD-mLvoJum~c ftask as directed in 15.1. Proceed to M8IIIIWtO R8pNtabIIty FleprodUCIIIIIiIy
!.S.1.3. F~. (iii..£ 173'") (Ra,£113'")
IS.1.3 COol tho solution to room temperature, dil\.1teto 1. M.,,,,,,,,, el8ItI18HI-iCo-SMo 0.020 0.005 0.007
volume. and tn~. Anow insoluble matter 10 .enle, or 2. Mareglng Iteel (NIST 58, 0.20!1 0.009 0.017
dJy.filter through a coarse paper and discard the first IS to 20 0.21 Mn) "
mL of the filtrate, before taking a1iquots. 3. SUdnI8.. 1te8124Cr.13N1 (NIST O.iDe O.DOS 0.016
.47, an Mil)
15.1.4 Using a pipet. transfer 10 to 20-rnL a)iquots as 4. 8181n1ea18teet 18Cr..oNl (NI$T 1.79 0.04 O.os
specified in J5. J two 5O-mL borosilicate glass yolumecnc 101.. 1.71 MtI)
flasks. Treat one POrbOll as directed in 1S.3. Treat the other S. SIIIInIeN tt8BI 1B.5Cf.t.SNI 3.31 0.05 0.11
(NIST 4.43, 3.38 MIl)
ponion as directed in 15.4.1. 8. 518W0II 8te81 2o.SCr-10Nl 4.80 0.04 0.13
15.2 Reagefll Blank Solution-Carry a Teaicnt blank (MST 444. 4.12 MIl)
through the entire prcx:edure usiJ:lgthe same amounts of all .. 'me tea( WI\8perfDmlll\lIn ~
. WilliIII. 1SeOwnIoII
0' PraoIICO
reagents with the sample om itted. EI73.
IS.3 Color Development-Proceed as directed in 14.3.
15.4 Referen.ceSolUlion:r: . PHOSPHORUS BY THE MOLYBDENUM BLUE
15.4.1 Backgrawad Color Solution-To one ofthc sample PHOTOMETRIC ME11{OD
aUquots in a SO-mL volumct.ric flask, add 10 mL of
nitric-phosphoric acid mixture, and heat the solution at not 18. &:ope
less than 9O"C for 20 to 30 min (Note 2). Cool. dilute to 18.1 This melhod coven the detennination of phosphorus
volume (with untreated water), and mix. in concentrations nom 0.002 to 0.35 %.
15.4.2 ReaCt!1lt Bltmk Rd'erence SDlutiOll-Transfer the
reagent bIauk solution (15.2) to the same size yolumetric
6ask as used for the test mlutions and transfer the .same size 19. Summary of Method
aliquo!$ a$ wed for the test solutioN to two S()..mL 19.1 See Section 19 of Test Methods E 350.
volumetric flasks. Treat one portion as directed in IS.3 and
use as reference solution for test samples. Treat the other as 20. Con~tration Range
directed in 15.4.1 and use as reference solution for Back- 20.1 See Section 20 atTest Methods E 350.
ground Color Solutions.
15.5 Pholometry-Establish the cell corrections with the 21. StahUity of Color
Reagent Blank Rererence solution to be used as a reference
solution for )Sackgound Color solutions. Take the photo- 21.1 See Seotion 21 of Test Methods E 350.
metric reaWngs of the Background Color Solutions and tbe
test solutions ycrsus the respective RCa&ent Blank Reference 22. Interferences
Solutions as directed in 14.4. 22..1 See Section 22 otTest Methods E 352.

16. Calculation %3. Apparatus

16.1 Convcn the net photometric reading of tbe: C,st 23.1 See Section 23 of Test Methods E 350.
solution and of the background color solution to milligtams
of manganese by means of tbe calibration curve. Calculate 24. Real(eI1b
the percentage ormangan~
Manganese.
as ronows:
... (A
'"
-
B)f(C)( 10) (I)
24.1 Proceed as directed in 24.1 through 24.7 of Test
Methods E 350.
where:
A '= manpnese, mi. found in 50 mL of the final test 2S. Preparation Dr Calibration ClII've Cor Concentrations

B . !olution,
apparent manganese, mg, founei in SO mL of the tinal
background color sojution, and
froID0.005 co0.05 .a/l00 mL
25.1 Proceed as directed in 25.1 through 25.6 of Test
Methods E 350.

t.opyright by the American Society For Testing de Katerials

Fri Sej) 18 13:~7:42 IS9a
 330 643 9076 P.06
ASTft E353 ~3 II D1S'S10 DS2SaSO 3T3..
4t e 353
26. Preparation of Calibration Cune for Coneeatrations 38. SUmm11JY of Method
from 0.&5to 0.30 me/l00 mL 38.J See Section 38 of Test Metbods E 350.
26.1 Proeeed as directed in 26.1 through 26.6 of Test
Metho~ E 350. 39. IDterfcreDCCS
39.1 The elements ordinarily present ao not iaterfcre if
27. ProceduJ"e their concentrations arc under the maxiU1umlimits shown in
27.1 Fo, Samples COfUaining Less rhQl/ 0.$ Tungsten: 1.1.
27.I.l Test Solution: "
27.1.1.1 For concentrations not greater than 0.30 percCJ1t 40. Apparatus
phO$phcrus, use a 1.0-. sample; for the concentration raage 40.1 See Section 40 of Test Methods E 350.
from 0.30 to 0.35 "pbospholU5. use a 0.85..g sample. Weigh
the sample to the nearest O.S ms. and transfer it to a 2S0-mL 4J. Reagents
Erlenmeyer flask. 41.1 Proceed as directed in 41.1 through 41.6 of Test
27.1.1.2 Proceed as directed in 27. 1.2 and 27.1.3 of Test Methods E 350.
Methods E 350.
27.1.2 Proceed as directed in 27.2 througll 21.S of Test 4%. Calibration
.
Methods E 350. 42.1 Proceed as di~cted in 42.1 through 42.6 of Test
27.2 For$amples Containing More Than 0.5" TUllis",,: Methods E 350.
21.2.1 Test Solution:
27.2.1.1 For concentrations not greatcr than 0.30 % phos- 43. ProaItIure
phorus, transfer 0.100-g samples, weighed to the nearest 0.1 43. t Proceed as directed in 43.1 and 43.2 ofiest Methods
mg, to two 10o..mL Erlenmeyer t1as1c1;for the concentration E3S0.
range from 0.30 to 0.35" phosphorus, transfer 0.085-g
S&nIptes,weighed to the nearest 0.1 mg. to two IOo.mL 44. Calculation
Erlenmeyer ftasks. 44.1 Proceed as directed in Section 44 of Test Methods
27.2.1.2 Proceed a$ directed in 26.2.1.2 "nd 26.2.1.3 of E3S0.
Test Melhods E 352.
27.2.2 Procc:cd as directed in 26.2.2 throu&h 16.2.5 of 45. Precision
Test Methods E 352. 45.1 Twenty-two laboratories cooperated in testing thii
method; six used resistance fUrnaces and reported eight sets
%8. Calc:wation of values (Note 3)~uteta. used induction furnaces (Note 4).
28.1 Proceed as directed in Section 28. Test Methods They obtained the data summarized in Table 3 for maleria1
£350. 7. Although samples covered by this method with sulfur
concenuation nCll' the lower limit of tbe scope were Dot
;Z9, Precisjol1 available for testing, the precision data obtained using the
29.1 Nine laboratoriC$ coo.,erated in testing this method methods indicated in Table 3 should apply. None was
and obtained the data summarized in Table 2. available to permit a test near the upper Hmit of the scope.
NOT& J- The recovery of suIfiar aa SO, r:maed ftalr! 7210 97 '1GIA'iIh
SULFUR BYTHE GRAVIMETRICMETHOD an aVCt8CCYllile of 83 buc:d an aallbMiGn staltdardilksiSllllled b. t.
aru1 d ill Table 3. "
(TbU method, which QODsisted of Sections 169 through Non 4- The recovery or sulfur u S02 rallaed froll'l 80 10 96 with
179 of1his sundard, was discontinued in J988,) in avcf1SC value of 88 based 011calibration naftd&rds desi'Dated" b, t,
aud d ill Table 3. "
SULFUR BY THE COMBumON-IODAT:E TI1'RA.nON
METHOD SILICON8V nm GUVJME11UCMEmOD

31. Scope 46. Scope

46.1 This metbod covers tbe determination of silicon in
37.1 This method covers the det.cm'lination of sulfur in
concentrations (rom O.OOS to O.S %. concenuations from 0.05 to 4.00 %.
47, Summary of Test Method
TA8LE 2 S&8tiatJqJ Iftformltloll-Pho.phOlH
47.1 See Section 47 of Test Methods E 350.
PI\oIpharu& RflpellaI)/Il!y~I)'
Tesl MlItIfaI F~. (A,. 15173-") (R2.E173AJ 48. Interferell",
1. Stahleu srAIeI 1ecr09NI (NBS 0.025 0.001 0.004 48.1 The eJements normally present do not interfere if
101.. O.02S P) \heir concentrations are under the maximum limits shown in
2. SlaInJ8sc ateeI 19C,.14Ni-3Mo 0.026 0.1!O2 0.004 1.1.
(N8$ 11OA.0.027 Pj
3. SlaInIeaa ltee! 17Ct-9NI~.~se 0.128 0.007 0.012
(NSS 3311.11.129P) 49. Rupr1t$
A TIllS leSt was pII/fCtIIIed In 8CX1111'0/ICI
willi Ihe 1980 v.~ of PractlCt 49.1 Proceed 8$ direeted in 49.1 tbrough 49.4 of Test
15173. Mtthods E 350.

terinls
 330 643 9076 P.07

AIT" E353 ~3 II D7S'S1D 0525651 23T ..

4t E 353

TABLE 3 S..II8Ucallnformatlon-Sulfur TABLE" Slallltlcallnfvnn.tkm-SllIcon

Sulfur R,,~ty $IIIeorI
R8p88l8IIIII" ~Iy
F~.
(RI' E 1'73'"
F~. (R,.E 173'" (R.. e 173")
Incluc;tign FIlfI18W HOIO. D.n~1icIn
1. NO. 1. 1:352 0.008- O.OOf' 0.0032 1. StllinltaS 111811SCr.9N1(NBB 0.428 0.014 0.021
2. No.2, 6352 0.0088 0.00 13 0.C!044 101e. 0.43 SI)
3. No.3. E360 0.014- 0.00:25 0.0029 2. $laInIaJs 11001IQcr.141\NMo 0./102 0.Of8 0.031
.. No.4. &360 0.01 B8 0.0018 0.0024 (NBS 160.. 0-605 SI)
5. No.6. e 350 0.032° 0.0032 0.0049 3. Sla!nIeIIlltII8I18Ct.1QNi.O.4T1 0.642 0.0'9 0.031
6. No.7. E350 0.141" 0.006S 0.0128 (NSS 1210. 0,64 II)
7. StaInIe&a&181II13Cr.o..1Mo 0.2"1! 0.0135 0.Q201
(HaS 1338.0.3299 + NBS,O HdO. C.hydrallon
Q. 0.109S: D.2'BS) 1. $JIllnltIUI88I18cr.9N1 (N8S 0.428 0.021 0,033
101.. 0.43 SI)
R.clcUll108 Fumat:18 2. $llIInlell steel 19Cr.14N1<3MO 0.60.1 0.017 0.014
1. No. 1. E3S2 0.0088 0.0014 0.D024 (NBS 1eo... 0.805 Sj)
2. No.2, Ii 3Ji2 0.0098 0.0007 O.GOaO 3. SI8lnleeleIHl 18Cr-10N100.4T1 0.&42 e.026 0.033
3. ND. 3. E3S0 0.0148 0.0014 0.0025 (MilS 121C, 0.&4 SI)
4. No.4. I! 3.50 0.0158 0.0017 0.0029 . ma Witwu D81f0lftl8cl /II~ wllh lIIe 1880 ver8b'I Of P'~1Oe
S. No. 6. UriO o.m" 0.0028 0.0041
e 113.
6. "0.7. &360 0.141)0 0.0074 0.0111
7. S~us,,'3Cr.o.3Mo 0.28811 0.0123 0.02011
(NI!IS1331. 0.329S + HISS COBALT U THE ION.!XCIANGE-JoOTENTIOMETRIC
10g. 0.109 $: O.ZIOS)
'J1'fRATiON METHOD
.. TNt \811 was ~".onnsa In lICCGt(la/lcewilli till 1980 sIcII of PraC1lce
E173.
I> CIIIlbr.1iotI .tanClarUS:
53. Scope
FooltlOle Tallie 5. M'Ithocls E 350.
e Cllllbrelion st8tlCl8rda:
S"
See F(IOtftat8
".
.. Tsblt 6. MaI/104' e 350. 53.1 This method covers tbe determination of cobalt in
I' CallbrIIIClll sl8ndanf1l: See FClDImI8 e. Table 5. Metf10ds e 350. concentrations from 2 to IS %.
~ CaHbraIloll staIII:Inl: SH Foomo18 0. T8b18 5, Mlllhadll E 35!t

54. Summary or Method

SO. Procedure 54.! See Section S4 of TestMethodsE 351.
50. { Select and weigh a sample in accordance with the
(ollowing: 55. Jnterrerences
Tolmauc:c in Dch~drnlill8 Acid, mL
55.1 The elements ordinarily present do not interfere if
Silicon.
Sam!!l; Simpl; Weiahl. ..~.
(I+4) tiOO.
their concentrations an: under the maximum limits shown in
Welahl.8 "'. 1.1.
"
o.OS 10 ..GO 4.0 4 ISO 60
1.00 (0 2.00 1.0 J 100 so 56, Apparatus
2.00 10 4.00 2.0 2 100 40
56.1 See Section 56 of Test Methods E 351.
Transfer it to a 400-mL beaker or II 300.mL porcelain
casserole. 57. Reagent.
50.2 Proceed as directed in 50.2 afTest Methods E 350 if 57.J Prcx:ecd as directed . in 57.1 through 57.4 of Test
tungsten is greater than 0.5 %. Methods E 3S 1.
50.3 Proceed as directed in 50.2 or 50.3 of Test Methods
E 350 if tunpten is Jess than O.S %. 58. ProceclW'e
50.4 Proceed as directed in 50.4 tbrough 50.6 of Test 58.1 .Proceed as directed in $7.1 through 57.6 of Test
Methods.E 350. Methods E 352.
50.S Proceed as directed in 5O.7 or Test Methods E 350,
but if the sample contains more Ulan O.S % tungsten, ignite 59. Calcu1atioD
at 750 C instead of !lOO to USO C afte.r volatilization of 59.1 Proceed as directed in Section 59 of Test Methods
Si02. E .351.
60. PrecisioJl
51. CnJaalatlon 60.1 Althougb samples covered by this method were not
S 1.1 Proceed. as directed. in Section 51 of Tcst Mc:thods available for tcsM,. the precision data obWncd for other
E 350. types of alloy$, using the methods indicated in Tab]e 5
should aPJlly.

51. Precision COBA.LT BY TIlE NlTROSO-a.s.u.T PHOTOMETlUC

MrnIOD
52. I Eleven laboratories coopentted in testing this method
and obtained the data summarized in Table 4. Samples with 61. Scope
silicon concentrations near the extreme limits of the scope 61.1 This method covers the determination of cobalt in
were not available for teSting. concentrations ftom 0.01 to 5.0 %.

I.opyright by t Amencan Society For TestiD& teriols

.
fr.i Sep 18 13:47:57]998 '"
 330 643 9076 P.08

AST" E353 ~3 II Q15'510 0525652 17b II

4~ E 353
TABU! S SIaUaUCIf IftfOl'lllltiO"-Cobail TABLE . SI8t1aUC8Ilnfonn811on-CObelt
CGb8/tFOUIId. ~ty Ae~bllly CoNII Found. ltepllll8tlNlly A8cw'adudbllcy
Tilt M S IR,. e 173AJ IRa. E 113.) Tel' MIII8'i5 S (R.. E 113AI (Ra.E 1)'SA)
1. No.1,Ean 1.86 0.05 0.12 1. No. 1. E 360 0.011 O.aos 0.001
2. No.2. e 11$2 4.82 0.0' 0.11 2. 51 , s188l.t7Cf-lNl(NSS 0.011" 0.004 0.0'3
SoNo.3. E 352 8.46 0.03 0.07 339. 0.098 Co)
4.No...e3~ 11.27 a.os 0.111 3. StIInI811 11881. 1 ICr-INI- 0.173 0.026
5. No.5. E3$4 13.88 0.09 0.18 O.26Se(NIS t01I,O.t8CoI
A ThIs 1811WH l*fomllCl III~ wilt!UIet980 of PrICtlce -.Ion .. Nil.4. eas. 0.468
5. StalrlIeSlltIII,1SCr-'5NJ.3Mo 1.01
0.020
0.04
0.028
D.oe
e 173. II.No.2. £352 '.87 0.01 0.13
'T. No.3. 1;:352 4.94 0.118 0.17
62. Summary o( Method &TIlls wa. P8tforrnect In 6CCOIdara with 11I81980 _siOft <I' ~
E173. '"I
62.1 See Section S4 of Tcst Methods E 350.

63. Conc:eDllatloa RaDle 71. Summary of Method

63.1 See Sec1ioD 55 of 1'est Methods E 350. 72.1 See Section 77 of TeSt Me1hods E 350.

64. Srabilll)' of Color 13. Concentration Ranle

64.1 See SeCtion S6 of Test Methods E 350. 13.1 See Section 78 of Test Methods E 350.

65. lQterf'eren~e8 '14. StablUry of Color

6S.1 See Section 57 of Test Methods E 350. 74. L See Seerion 79 to Test Methods E 350.

Reagents 75. Interferencu

". 75.1 None of'thc clements usually present interfere jfth~r
66.1 Proceed as directed in 58.1 th10Ugb .58.4 of Test concCntnl.tioM arc under the maximum limitS shown in 1.1.
Methods E 350.
16. Ap,aratus
67. Preparatioa of Calibration Curve
76.1 See Section 81 of Test Metbods E 350.
67.1 Proceed as directed in 59.1 Ihrough 59.S of Tcst
Methods E 350. 17. Reagents
77.1 Proceed as directed in 82.1 throuch R2.9 of Test
68. Procedure Methods"E 350.
68.1 Test Solution:
68.1.1 Proceed as directed in 67.1.1 tbrouch 67.1.3 of 78. Preparation of CaUbntJon Curve
Test Methods E 3S~. 18.1 Proceed as directed in 83.1 through 83.6 ot Test
68.2 Proceed as directed in 60.2 tbrough 60.4 of Test Methods E 350.
Metbods E 350.
19. Procedure
6'. Calculation 79.1 Ptoceed as directed in 84.1 tbrQugb 84.~ of Test
69.1 Proceed as directed in Section 61 of Test Methods Methods £ 350.
E350.
80. Calculation
70. Predsio09 80.1 Procced as directed in Section 85 of Test Methods
70.I Eight laboratOries cooperated in :\ming tbis method E3S0.
and obtained tbe data summarized jn Table 6 for materials 2,
3, and 5, Although samples CO\Ieredby this method witb 81. Precision
cobalt concentrations near tbe ex~me limitS of the scope 81.1 A minimum of'eiJbt laboratoriescooperated in cesting
were not available fOt tesnD&. the precision data. obtained for this method end obtained the c1atasummarized in Table 7,
ether typeS of alloys, using the methods indicated in Table 6
should apply. TABLE7 St8t1at1ca1lnlorm81k111-Aluml"um
Teat Material
AlUmInum Reputability R8P'~1Ity
TOTAL ALUMJNVM BY mE 8.qUINOUNOL Folllld., (R,. e f73AI CAa.E f73.'
PHOTOMETRIC MtTHOD 1. Type 3D4 5t8/11111Stsl88l 0.004 O.DO' 0.003
1ecr"NI
11. Scope ~. 1}oP8~ 8t81n111lltlll 0.045 0.008 o.ot 0
7 1.1 This n1cthod covers the determinauon' of total alu- tSCr"NI
3. Type304 Ninle81 _.. 0.083 0.004 0.009
minUMin concentrauons from 0.003 to 0.20 sri. ,BCr.8N1
4. ~ AZ8Ial8lnleSas\tel D.t9 O.Ot 0.Q4

10%7.
J
S\IPPO,,;nl dell 11IIIa'tailablc r,om ASTM HcadqlllftelS. IhC/wCiSllUC.:iOJ. .
t SCr.28N1

e173.
TN. 1851 was perf4/ftlOl! In IICOOfCf8nC.8with tile f980 vMtion of Pra;11C8

J 7

CO}lmmt 'by lhe American SocIety For TesUq &

Fn ~ei 18 13:48:04 1998
 AS"" E353
COPI'U IY THE SULFIDE P1tEClPITATION.
EUCTRODEPOsmON CRAVJMETlUCMmlOD
82. Scope
82.1 This method covers the determination of copper in
conceutratiODi from 0.0 I to 5.00 %.
83. SummlU')' of Method
83.) Copper i.sprecipi~ated as the sulfide rrom dilute acid
containing chloride and nitrate ions. AI'teJ'dissolution of the
precipitate, iron is added and tin is Iepara1ed from copper hy
double precipitation with ammonium hydroxide (Note S).
CbIoride ions are removed from the filtr'gU, and copper, as
the metal, is deposited on a platinum cathode.
Nor!! 5- This merhocl dcsaibes &he pre1imina.ry scpInatioll$ For tbe
dClcnnination 9f tin by rhe sult1de-ioclalimouic 1ilnltioa melhod.
84. Interiereneu
84.1 Ammonium salts may cause the copper deposit to be
spongy and subject to air oxidation wbile drying in the oYen.
If this occurs the cop-per should be dissolved from me
platinum cathode and redeposited (Note 8),
85. Apparatus
85.1 Apparatus No.9.
86. Reqents
86.1 Ammonium SuU'ate-lfydl'Ogen Sulfide $ofutio1l-
Dissolve 50 g of ammonium sulfate «NH.hSO..) in about
SOOmL of H2S04 (I +99), dilute to ] L y~th H2S04 (1+99)
and saturate with bydrogen sulfide (H2S).
86.2 Ferric Chloride Solution (2 g Fe/L)-DiJsolve tOg of
ferrie eh]oriciehexahydtate (FeCl).6H10) in about 800 mL
of Ha (J+99) and dilute to ) L with HCI (J +99).
86.3 Sul{amic Acid (H<NH:JSOJ).
87. Procedure
87.1 Sel~ and weiab a sample in ao:ordancewith the
foUowin8:
Toler'BIZ in Sample
~. Sample
We;"",. WcWll,m,
"
0.01 101.0 10 10
0.0 10z.j S S
2.5 10$.G 2 2
Transfer it to a t-L Erlenmeyer flask.
87.2 Add liS mL of HCJ (1+2) plus an addiLional 9 mL
ofHCI (1+2) and J mL or HN03 for each gram of sample.
Heat until diS$OJution is complc:te, and then boil the solution
COt2 to 3 min. If the solution i$ clear, proceed as directed in
87.3 and 87.8 through 81.21.
81.3 Caay a reqent blank through tM entire procedure
using the same amounts of all msgcnts with the sample
omitted.
87.4 If toe solution conuin& insoluble maner, add paper
pulp, digen 1S to 20 min, and then fiher throu&h medilnn
filler paper into a I-L Erlenmeyer tJast. Stlction may be used
if ncc:essatY. Wash the filter 4 or 5 times with water. Reserve
the filtrate. Proceed as cUrectedin 87.4.1 (or 81.4.2 according
to preference. bearinc in mind that th~ latler procedura may
be the eii5icr to apply when copious aJn'ountS of insoluble
matter are cneOJADwed.
Copyright by lhii American Society for
Yri Sep 18 13:48:12 1998
!lf3 .
4~ E 353
075'5]'0 D525653 D02 .330 643 9076 P.
81.4.1 Transfer the I'8per and precipitate to the original
l1ask, add 20 mL of HN03 ane! 10 mL of HOO.. heat
moderately 10 oxidize organic: maUer. and finally heat to
mild fumes of HCIO,. Cool the !lolurion, add I to 2 mL of
HF, and Mpe.atthe fUmiq.
~.4.2 Transfer the paper and precipitate to a platinum
crucible. DIy the paper and heat at 6OO"Cuntil the carbon is
removed. FinaJly isnite for 30 min at l IOO.C.Cool, add 3
drops of HNO, and I to 2. mL of HF. and evaporate to
dryness. Add 10 mL of HNOJ (1+1) and digl!$tat 90 to
lOO'Cior 5 min. Transfer tbe contents oCthe crucible to the
original Oask.add 10 mL otHOO... and heat to mild fumes
of HOO,.
87.S CooI1besolutionfrom &7.4.1 or 87.4.2, add 100 roL
of water and digest at or near boiling {or about 45 min.
87.6 It'tUDgsten is present, as in4icated by the presence of
a bright yellow precipitate oftulIgstic acid, add a slight c::x.cess
ofNH.OH and 20 g ofurtaric acid. When 1he tat1arie acid
has dissolved, again add a slight CXces!ofNH,.OH and digest
near the boiling point until dissolution is complete, or neatly
so.
87.7 Add 5 mt otll~O. and heat at 85 to ~WC for 30
min. If insoluble matter persists, repeat the steps as Qirected
in 87.4 through 87.1. When dissolution is complete, combine
the solution with the filtrate reserved. in 87.4.
87.8 If the volume is less than 600 mL, dilute the solution
approximately to that volume and treat with H2S: admit the
gas at Q.rate sufficient to cause a Steady stream of bubbles to
leave tbe solution. Continue passins the ps into tbe solution
for at least I h. Allow to stand until the supernatant solution
becomes clear, but not longer than 12 to ISh.
87.9 Add papet pulp and fi]tcr using a fine titter paper,
Wasil tile filter thoroughly with ammonium sulfate-hy-
drogen sulfide wash solution. Discard the filuate.
81.10 Transfer the mter paper and precipitate to the
original flask. add 12 mL or H2SO... and heat to char the
paper. Add 20 mL of HNOJ, and evaporate to fumes to
destroy organic matter. Ad<i HNOJ in l-mL increments and
heat to fumes after each addition to oxidize the last traces or
organic matter.
81.11 Cool the solution, rinse the sides of the flask. and
repeat the fuming to ensure the complete removal ofHN03.
87.12 Cool, add 100 mL or water, and boil to dissolve the
soluble salls. Add IS mL of HC/, and digest for about 10
min.
87.13 Filter through 4 coarse tiher paper into a 400-mL
beaker. Wash the filter altemately with hot water and hot
HCI (1"'99). Discard tbe filter paper_
81.14 Add 10 mL or FeCI] solution to the fIltrate. Add
just enough NH..OH (1+ 1) to precipitate the iron, tin, and
chromjum and to complex the copper (indicated by the
(ormation ora blue color), and then add I to : mL ill ~cess.
Acid paper pulp, and heat the solution 10 boilinS te coasulate
the precipitate. Filter the hot solution through a coarse ftltet
paper, and wasb alternately five tiJnes eacb witb hot NH,OH
(1+99) and water into an 800.mL beaker. Resel"l/c the filter
and the fUtrate. Dissolve me precipitate by washina tbe mter
alternately with ho1 RCI (I + 1) and bot water, and Te$Crve
the filter paper. P.redpitote the iron. tin, and chromium as
before. Wash the rCSCl"I/edfilter paper thrcc: times with hOl
NH"OH (1"'99) and tben fIlter the hot soludoll into the
 330 643 907t: P.Ol
AST" £353 ~3 .. a7S'5~U U~~~eb~ U~~ ..

4t E 353

tr.msfer a 20-mL aliquot to a 600-mL beaker. and dilule to 181. Silmmarr oJ Metbod
100 mL wi~ water. l8U tin is extracted from a dilute hydrochloric ;t~id
177.3 Add 10 mL of ammonium citrate solution and 10 solution of the sample, c:ontaudag ascorbic acid and ];)Otas.
mL of HCI. Using a pH meter, adjust the pH to at lea.st 1.5 sium iodide, into a solution of trioctylphosphinc oxide
with NH.OH. Remove and rinse the elcctrodCl with water. (TOPO) in methyl isobutyl ketone (MIBK). The MIBK
collecting the rinsinss in the original beaker. ~11'a<:t is aspirated into the nitrous oxide-acetyJene fll!me.
177.4 Add 2 mL of HCi and. while stirring the solution. Spectral energy at 2863 A from a tin hollow.catbodc lamp or
add 10 IQL of dimethytslyoxime solution plus aD additional tin electrodeless discharge lamp i5 passed through the l1ame
0.4 mL for each milJ.i.sram ofDickel present If the separation and the absorbance is measured.
was made by anion-exchangc. add an additional 0.4 mL for
each miltigram of manganese prtSCnL 182. Conc:entrlltion Range
177.5 Usins a pH meter, a(ljuSt the pH to 7.4 :1:0.1 wiLh 182.1 The recommended concentratioll range is from 4 to
NH,OH. RemoYc and rinse the electrode with water, Heat at 20 jLgoCtin per milliliue in the final 10 mL orTOPO-MIBK
SOto 70'C for 30 min and allow 10 srand ror at least 4 h at 20 extract.
to 25.C.
117.6 Wilh tbe aid of suction, filtEt using a weighed (Note 183. Interferences
24) fritted glas,s crucible, wash the beaker and precipitate 6
times with cold water. 183.1 Copper. when present above 0.1 8. interfr:r'!:1\by
precipitatiDg as cuprous iodide (CuI). This interference. may
NoTII 24-Heat the cn&I:&'b1cat I SO'C. and 1:001 in a dc&ic:c:ator before
be elimina.ted by incorporating Ii suitable copper sepaJ'1\itlon
ftiabioa. scheme into the procedure prior to the solvent extrat1.ion
177.7 Dry at I SO'C at least 3 h to ~onstan\ weight. Cool in step.
a ~ccator and weish.
184. Apparatus
118. Calculation
184.! Atomic AbsorPtion Spectrophotometer, capable af
178.1 Calculate 'he percenta&e of nickel as foUows: resol¥.ing the 2863 A line, equipped with a. tin hnliow.
Nickel," - (A - B»)( O.2032/C x 100 (13) cathode lamp or tin elcdrodeless dischar&e Jamp whose
where:
A .
weight of CfUcible anci precipitate, e.
B = weight of crucible, it and
radiant energy is modulated, witb a deteCtorsystem tuned to
me same frequency and a premix nitrous oJtid~ceiyJene
burner. The perf'orman~ of the instrulDent must be "uen
C = sample, B,represented in the final test solution. that me Ul'per limit of the concentration tanic (40 ilg/rnL)
produces an absorbance or o. IS or bisher. and a calibri.\tion
curve wbose deviation from linearity is within the hmits
179. Predsioo4 specified in 186.4.
179.1 Nine laboratories cooperated in testing this method
and obtained the data summari2ed in Table IS. Although J 85. Reagents
samples covered by this method near the lower and upper 185.1 Ascorbic Acid.
ends oftbe sco~ were not tested. the data obtained for other 185.2 /od.'de-AscorbicAcid Solution-Dissolve 30 iJ,or
types of alloys usifll the methods indicated .in Table IS potassium iodide and 10 &or ascorbic acid in 60 roL or HCl
sbould appJy. (I+S). Dilute to 100 mL with water and mix. Do no! use a
solution that has stood more than one da)'.
TABU 15 Slarlatlcal'n'armatJon-Nlckel 18S.3 Methyl Isobutyl Ketone (MIDI<).
NICk8I A~lIly 185.4 Tin. $randard So/urion A (I mL"" 1.0 mg 511)-
Found. (R.. RlprocIvCIbIIIty Dissolve 1.000 g oftm (purity: 99.9 % minimum) in IDOmL
1'lIIt Malsr181
e 173") (R~.E 173")
s of HCl. Cool, transfer to a I.L volumetric nask. dih.\te to
1. ND. 1, E352 0.135 0.012 0.016 volume with HCl 0+2). and mix.
2. "'I;h c:/VOIIIJ\IIII'\HI
'3
Ct 0241 0.019 0.018 liS.S Tin, Standard SoIlIl/on B (1 mL]II; 50.0 J.I&SI'I)-
(NBS 73c. 0.2.. NI)
3. StaInItsa IIt8II ,. Cr-I N~25 9.44 0.14 0.25 Using a pipet, transfer a JO.mL aliquot of solution A !o a
Sf (NBS 1018.9.48 Nt) 2()O..mLvolumetric flask. Dilute to volume wi1h RCi i +2)
,. at_,O Cr.1. N~3 14.11 0.26 0.31
S"~8 and mix.
Mo(NBS 180..14.13 Nt)
5. No.4. E364 20.28 0.23 0.17 185.6 Trioctyfpho3phine Oxide (TOPO-MIBK) So!wion
II. ND.Ii.E~ 77.13 a.sa Q.$5 (50 gfL)-Transrcr 12.5 g of TOPO to a 2S()..mL volum~tric:
..ThIs test was pufonneCIlI\ IICCQIUaIIc:I
WIt/!UI81980 versllJnor ~ ftask. Dilute to volume with MIBK and mix. until dissoJution
E173. is complete.

186. Preparation of CatibratlOD Cune

'I1N BY mE SOLVENT EXTRACI10N-ATOMIC
ABSORPnON METHOD 186.1 Calibration Solutions-Using pipets, tcansf~! 0, I,
2,4.6, and 8 mL of solution B (t mL"" SO ~8 Sn) to IOO.mL
ISO. Scope volumetric flasks.
180.1 This method covers the determination of tin in the NOT!! 25-Voilimettic Rasia with &rQund &low stoppe'" m:.L,t be
range from 0.002 to 0.10 %. used..

17

Copyrig t by tbe America4 Soeiely or Testiug Ie Materials

Fri Sep 18 13:49:30 1998
 330 643 907"
AS Tn £353 93 II 07h~~~u U.3C.:Ioa-J IJ..._ P.02

~ 186.2 Extraction:
.
186.2.1 Add 15 mL or HCI (1+ I). 3 g of ascorbic acid.
and mix, Add 1S mL of iodide-ascorbic acid solution. adjust
the volume to approxim~ely 50 rnL, and mix.
186.2.2 Using a pipet. add 10.0 mL of TOPO-MIBK
solution, stopper the flask, invcrt. and shake viaorously
several times for a period of I min, Allow the phases to
separate. Add water to brina tbe entinl ol'lanic layer up into
the neck portion of the flask. Stopper, invert s~raI times.
and allow the pbases to separate.
NOT!!26-Pr'PIte lIIe test solution and have it ready to aspirate
immediately after 15Piralins the calibration. 5OIudolU.
186.3 Photometry:
186.3.J With a tin hollow-ca.thodeJamp or electrodeless
discharge lamp in po$ition, energized and stabilized, adjUSt
the wavelength.settina to the location that gives tbe max-
imum detector respon!e in the immediate vicinity of 2863 A..
186.3.2 Following the inStrument manufacturer's specific
directions, ignite the burner U$ins the air-acetylene mOde of
operation. Immediatety after ignition, switch over to the
nitrous oxide-acetylene mode of operation and allow the
b~rncr to reach wnna1 equilibrium while aspirating water.
Ca.utiously adjust the height of the red cone of the flame to
approximately 12 mm by means of the fuel now needle
valve. Adjust tbe detector response to zero while aspirating
waler.AspirateSolutionB (I mL ~ 50JigSo)and adjustthe
height of the burner to obtain maximum response from the
detector system. Remove the capillaty from the solution
allow air \0 aspirate ror 15 to 30 s. Aspirate MIBK for 30 s.
then readjust the detector response to zero, if necessary.
Non; .17-From tlUs r>oint on. only MJBK ,elutions sbouJd be
aspirated UII\IIalllC1t "lid calibration solution measurementS have bceII
completed. If the burner slot shows an)' 5ign of blocb&e, 5b1J\olT the
name accordins \0 the innnnl1cnl rnanuCacturer's approved procedures,
clean the slot, and ~Ii&ht as in 116.3.J.
186.3.3 Aspirate the 5Ohnion with the highest concentta.
tion (40 \18 Sn/mL) from the series prepared in 186.1, a
5\lfficienl number uf times to establish mat the absorbance
not drifting.
Non 28-Mak.e certain that the capillary end does nOLenter the
aquoous (bollOm) layer at any time.
NOTE 29-Duc to the :small amO\1nt or tXtract available for makinJ
this test, tJlI~numbct of~adinB5 and the lime between readinp m\l.Stbe
bpI Laa minimum.
186.3.4 Beginning witb the calibration solution to which
no tin was added, aspirate each calibration solution in turn
and record its absorbance. If the value for the solution with
the highest concentration (40 IJ.SSn/mI..) differs from tbe
average values obtained in 186.3.3 by mon: tban 0.03
multiplied by the average oftbr; valur:5, repeat the measure-
mcnt. If this value indicateS a trend or drift, detennine the;
cause (for cxample, depoat in the burner or clogged. capil-
lAry), correct it, and rCl'ea.t the procedure in 186.3.1 through
186.3.4.
186.3.5 Proceed immediately as directed in 187.3.
186.4 Calibration Clll'Ve-Plot the average ntt absorb-
ance values against micrograms of tin per millititrc on
rectangular coordinate paper. Ca.1culate the deviation from
linearity of tbe curve as follows:
DcviatiQn from linearity - - 8)/C
(A
o E 353
where:
If ... absorbance value for 40 ~g Sn/mL,
B ;: absorbance vahlc for 30 Jil So/mL, and
C -= absorbance vaJue ror 10 1 Sn/mL..
lCtbe calculated value is less tbaft 0.60. comet the indicated
ma!.fupctiol1, or maladjustment of the instnunent, or bim p.
and repeat lhe calibration.
187. Procedure
187.1 Reagent Blank-Carry a rugent blank through the
entire procedure using the same amount of all reagents wl::h
the sample omitted.
187.2 TeJt Solution:
187.2.1 Select and weigl! a sample to thenearcst 0.5 mg in
accordance witlt the foltowing:
Tin, ~ Sampl; Weiahl,8
0.002to 0.005 3.00
0.004100.010 2.00
0.009100.050 1.00
0.045to 0.100 0.50
Transfer it to a 2S0-mL poly(tetrafluoroetbylcne) beaker.
187.2.2 Add 100 mL of HCt (1 + I), to drops of 30 ';:;
H20.1' and S drops of HF. Cover the beaker with a
poly(tetrat1uorocthylcne) cover and heat at a low ttmper,,-
tUfe (appro"ima~ly 90"C) unlil dissolution is complete,
NOTE 3D-ror sam\: Stcc15, it wiU be 1I~ to perioOically add ~I'J
and additional 10 drops of ~o" H20a to halten the dwoluugn oC th~
so.mgle. IfsiUcon is above O.S %, use to (012 drops ofKF.
187.2.3 Remove the cover with platinum-upped tongs
and cautiousiy rinse into the beaker with water, Cauuous!y,
evaporate the solution at a low temperature (approximately
90.C) to IS mL. Rinse the sides ofthe beaker with water, add
20 mL HCl (I + t), and again evaporate to 1S mL. Rinse; the
sides of the beaker with about 5 mL of water and cool.
187.2.4 Add 3 g of ascorbic acid for a I-g sample, plus:; g
of ascorbic acid for each additional I 8 of sample. SwirJ to
is dissolve. Add 15 m.L oIthe iodide-ascorbic acid solution.
187.2.5 Transfer the sampl~ to a lOO-rnL volumetric f!a:;k
and adjust the volume to approximately SO mL with wal.!':,.,
Using a pipet, transfer 10 mL of the TOPO-MIBK solu!icm
to the t1a.sk, stopper, invert. and shake vigorously severa]
timC$ (or I min.
181.2.6 Allow the phases to separate. Add water to bm'1g
tbe entire orpnic layer into the neok of the ftaslc. Stopper.
invert several umes. and allow tbe phAses to separate.
187.3 PhOlometry-Aspirate the top (M[BK) phase of ,he
test solution and the reagent blank solutioD (Note 28) and
record the absorbance values. Take three readinp of each
solution (Note 29). Meuure the absorbance of the calibr",.
tion solution with the highest concentration of tin to ched:
for drif\ as in 186.3.4 and 186.3.5.
188. Calculation
188.1 Convert tbe average absorbance ofthe test and the
reagent blank solutions 10 micrograms of tin per millili tre :;If
the final solution by means of the calibration curve. Calcu.
late the percentage of UD as tollows:
Tin, - {(D - E)/(F x 1000)J (1.'5)
(14) where:
'"

18

CopyrighL by the American Society For TQ!!tiDgat )Is. erial~

rn S!!P 18 13:49:40 1998
 16:15
ASTft E353 ~3 II D1~~~~U U~~~Ob~ ..u _ P.03

4~ E 353
l'AeLE 18 Statl,veal Inform.dolt- TIn NOTE 31- ThiJ ~ethoc1 has been written for cells havillJ !I! ",,:11
uab'
TIn path. Cells baving other dimeBSions may be used, -provide,d 5uiuble
Rtpea1811f111y Reproducilllllty adjulI&mPlScan be made: in the: amoun" of sample and r~ser,l.s used.
FCUIICI.
S /19,. e 173.) (R.. E 173.)
193. StabUtty of Color
,. No. 1. E35C
2. SIaInIIIt,reel.~
(1SC1'1
0.005 in (fa
.,,
eenifted)
0.003'
O.M4.2
0.0006
0.0008
0.0007
0.0011 193.1 The color is stable for at least 2 h; hcwever,
3. No. 2. E 350 0.0079 D.OOO9 0.001.
photometric readings showd ~ taken promptly occausc of
4. SIllln18s8 ._. 1')'P8 $1 & 0.006& O.OIIOS 0.0014 the volatite nature of the solvent.
(18Cr-13N}.2Mo) 0.008 Sn (not
atnIfI8d) 194. Interferences
5. S 8"". Type 0.017 0.002 0.004
(13Cr-10N1)0-017 8ft *(not t94.1 The ellmleDts ordinarily present do not izw:rtere if
0II1III8d) their concentrations are under tbe maximum limits $liOWnin
G. No. &.usa 0,097 0.011 0.011 1.1.
.. Thl. I.et was performed In IDOIIfdIIMI wIUI lite 11&0 YeI8iOn of Ptlctlce
E173. 195. ReageDts
195.1 BUlf/ Acetate:
D -
tin. j!g, !)ef mL of the final test solution. Non 32-()pcra1.i0tlS With tbis chemical mOllld be catrie.~ ;)\;t away
E - un, ~ per mL oCthe final reagent blank solutioa, and from heat aDd OpeD &mil ud arc best done in II wc:)1ventiJill.ed hood.
F os sample\I~d. g. Avoid prolon&ed brcathiD8 of vapor.
195.2 DissolvingSolutiolt-While stirring,add 300 mL of
189. PreclslOlland Biaau 8JPO, and 300 mL orHNo) to 1400 mL of HCIO(.
189.1 Precisiorr-Elcven laboratories cooperated in 195.3 lronl3-purhy: 99.8 % minimum. molybdenum
testing this method on No.2, 4, and 5 in Table 16. This 0.001 % maximum.
method differs only sJishtly from the method for tin Test t95.4 Iron SolWlionA.(I mL" 70 mg Fe}-DissoJve 2S g
Method S 350. in that the amounts of reagentS used to or feme sulfate (Fe:(SO..)3.9H20) in 75 mL of ho~ water_
dissolve the $IUt1pleswere increased. The fact tbat the Cool and add 10 mL ofH~SO.. Cool, and dilute to 00 mL.
precision of No.2, 4, snd S in Table 16 ccmespond closely -
195.5 /r01l Solution B (l mL 0.84 m&Fe)-Add 12 mL
with that obtained for the samples of similar tio content of ofironsolutioDA to 17$mL ofHzSO. (I + I), and dilute 10
Test Method E 3~O sugcsts mat the precision of the two IL.
methods is the same. 195.6 Molybdenum, Standard SolUtion'" (I mL "'.0.2 mg
189.2 Bia.s-No int'ormatioD on the accuracy of tbis Mo)-Reaseftt No. 8A, or 88, P~ces E SO.
method is available. The accwacy of the method may be 19S.7 Mo/ybde1lum.Standard Solution B (I roL 0'< 0.1 m~
judged. bowever, by comparing accepted reference values Mo)-Using a pipet, uaasfcr 50 mL of Molybdenum Solu-
with tbe arithmetic lYeI'aIC obtained by interlaboratory tion A 10 a lOO-mL vol\Jmetri~ ftask, dilute to volume, and
tcsting. The valllCS listed for tbese samples, while not mix.
certified,were obtained by other methods and are believedto 195.8Molybdenum, Standard Solut.iofl C (l mL ."" 0.01
~ substantially corTee\. mg Mo)-Using a pipet, transfer 10 mL of Mo!ybdenum
Solution A to a 20o-mL volumetric flask, dilute to' volumc,
MOLYBDENUM B\' THE PHOTOMETlUC METHOD IInd mix..
195.9 Sodium ThiO&)JtI1IQte SolUtion (100 g/L)-Re3gent
190. Scope No. 137, Practices E SO.
195.10 Stannous Chloride Solution (350 g,fL}-.Iransfer
190.1 This method covers the determination of molyb- 350 g of stannoua chloride dihydrate (SnClz' 2H20) and 200
denum in coDcenuaUOI\$ from 0.01 to LSO %.
8 oCtartaric acid to a I.L beaker, add 400 mL of H C1 (1 + I),
and heat at 60 to 10.C until dissolution is comJ)J~t,;;.Cool,
191. SWIUIt&ryof Method and dilute to 1 L. Add several pieces of tin. and $'lore in an
191.1 The test solution is treated with thiocyanate to air-tight bottle.
develop the molybdenum aDd iron thiocyanate complexes. NOT!! 33-Tbia soIudctl is wed. for color deve:loprneni in 196.3.
Molybdenum and iron are reduced with stannous chloride, 197.3, 198.3, aDd 199.3. WheII all absorption cell is uild &equcri~alIy for
and the molybdenum complex is extracted with butyl a tI\I.IIIber ofpbotomctric ~t1Iu, a white rum oraa in:>oluble tin
acetate. Photometric; mea.surcment is made at approximately ~mpoutld may aclb.ere to the inside or the ceU and mllU i;!(; remoV«J
berOft further measwemnu ate made.
475 om.
196. PrepatitloD of Calibrttlon ellfve for Conci?:utr!ltiOAS
19~_ Conceutradon Ranae from 0.01 to 0.05 %
192.1 The recommended concentration range is 0.0003 to 196.1 Calibration So/wions:
0.003 mc of molybdenum per milliliue of solution usins a 196.1.1 Transrer 0.3 g of iron to each oCrOYf250-mL
l-cm celt. Erlenmeyer flasks. Using pipets, transfer 2, S, 10, and 15 mL

II Suppord., ~ an: .wi'-blc rlOm A$TN H~8dqualtelS. ll!4ueR 'IUl:EOJ. U Joh_MatlJlcy JMC 147 IpOIlJe if\'\~ II.. been tOIiM .ui",~le for Ih~
1022. ptItpOIe.

19

Copyrigll by the American Society or Testtog bterials

VriSep 18 13:49:47 1998 "
 lb;lb
4SfIt
~of Molybdenum Solution C (I mL =' 0.01 mg Mo) to the
'1asks. Add 30 ml.. of dissolving $oluiion and beat until
JissoJution is complete.
196.1.2 Increase tbe.temperature and evaporate to HCl04
fumes. Coot, add SOmL ofwatcr and 70 mL of H2S04 (1 +
1).Heat to boiling and cool in a water bath.
196.1.3 Transfer to a 200-mL volumetric flask, dilute to
volume. and mix. Proeeed as directed in 196.3.
196.2 Reagem Blank Sollllion- Transfer 0.3 g ofkon to a
2SO-mL Erlenmeyer {task. Add 30 mL of dissolving solution
and heat until dissolution is complete. Proceed. as directed in
196.1.2. 196.1.3. and 196.3.
196.3 Color Developmenf-Usinc a pipet., transfer 100
rot to a 2So.mL separatory funnel. Add in order, mixing for
15 s after each addition, 15 mL ofNaSCN solution, IS mL
ofSn02 solution, and 25 mL of butyl acetate measured with
a pipet. Stopper and shake vigorously for 2 min. Anow the
pl\ase$ to separate, remove the stopper. drain on: and discard
the aqueous phase. Add to \he fUlmel SO mL of H2SO. (I +
6), S mL of NaSCN solution. and S mL of SnQa solution.
Replace the stopper and shake vigorously for 2 min. Allow
the phases to separate, remove the stopper. drain orr. and
discard the aqueous phase. Drain CftO",gJIorthe butyl aceta1.e
layer mrough a funnel conwning a dry filter paper to fill an
absorption cell.
NOTE 34- This funnel should be cleoanc.d lhoroucJtly 3t\ct each
IiImtioli 10 avoid developmtnt oh pink color Ihat would cQnl2immalc
lhe mUate.
196.4 Reference Solution-Butyl acetate.
196.S PllO,tlnaelry:
196.5.1 Multiple Cell Pholomeler-Measure the Telgent
. blank (which includes the cell correction) using absorption
cells with a l-em light path aDd a light band centered at
approximately 475 nm. U$ing tbe teSt ceU, take the photo-
metric readings of the ~'bration solutions.
196.5.2 Single Cell Photometer-Transfer a suitable por-
nODor the reference solution to an absorption cell with a
1.cm li~t path and adjust the photometer to the initial
settinz, using a light band centered at apwoximately 475 11m.
While maintaining mis adjustment, take the photomttric
readings of Ule calibration solutions and the reagent blank.
196.6 CalibrationCW'Ve-Plotthe net photometricread-
ings or \he calibration solutions against milligrams of molyb-
denum per 25 mL of butyl acetate.
197. Preparution or OalibratioD Curve for Con.ceotratioD'
from 0.05 to 0.S5 IVo
197. I CtllibraJion Solutions:
197.1.1 Transfer 0.3 g of iron to each of four 2S0-mL
Erlenmeyer flasks. Using pipets, transfer 2, 5, 10. and 1S mL
of MOlybdenum Solution B (1 mL 0.1 10; Mo) to the
nasks. Add 30 mL or dissolving solution"" and heat until
dissohltion is complete.
197.1.2 Increase the temperature and evaporate to RClO..
fUmes. Cool. add SO mL of water and 70 mL orH2SO. (1 +
1). Heat to boiling and cool in a water bath.
197.1.3 Transf'er to a 50Q-mL volumetric flask. dilul.e lo
volume. and mix. Proceec;l as directed in 197.3.
191.2 Reagent B/tJnk So/ution-Traflsfer 0.3 g anron to a
2S0-mL Erlenmeyer flask. Add 30 mL of dissolving solution
Copyright by lhe American Sociely for Tesling & Materials
Fri Sep 18 13:49:57 1998
330 643 9076 P.04
U :11:...""' --
e 353
and heat unlit dissolution is complete. Proceed as directed in
197.1.2, 197.1.3, and 197.3.
197.3 Color Development-Using a pipet. tranfler SOmt
to B2~()'cnL separatory tUnnel. Add in order, mixing for [S
s after each addiuoD, 15 rnL of NaSCN solution. 15 mL of
SuCI2 solution, and SO mL of butyl acetate measured with a
pipet. Stopper and shake vigorously for 2 min. Allow the
phases to separate, remove the stopper, drain on: and discud
the aqueous phase. Add to the funnel 50 mL of H2S04 (1 +
6), S mL of NaSCN sotution, and 5 mL of SnC11 solution.
Replace the stopper and shake vigorously for 2 min. Allow
the phases to separate, remove the stower, drain off, and
discard the aqueous phase. Drain enough ohbe butyl acetate
layer throush a funnel coataining a dry filter paper to fin an
absorption ceU.(See Note 34.)
197.4 Reference Solution-Butyl acetate.
197.S Photometry:
197.5.1 Multiple Cell Photometer-Measure the reagent
blank (which includea the cell corre<:tion) using ab$Orption
cells with a l-cm light path and a light band ~ntered at
approximately 475 nm. Uiing me test cell, take the photO.
metric readings of me calibration solutions.
197.S.2 Single Cell Photometer-Transfer a suitab1epor-
lion of tbe reference solution to an absorption cell with a
I-cm light path aDd adjust the photometer to the initial
settin&,using a lid1t band centered at approximately 475 nm.
While maintaining this a4justment. take the photometric
readings of the ealibl'aUODsolutions and the reagent blank..
197.6 Ca/ibra,ion Cunre-Plot the net photometric read-
ings of the calibration $OlutionsagainStmilligrams ofmolyl>-
denum pet SOmL butyl acetate.
198. Preparation of Calibration Cun'e Cor Coneenlrationt
from0.40 tl) 1.50 %
198.1 CalibrfJIionSolutions;
198.1.1 Transfer 0.3 g of iron to each of five 250-mL
Erlenmeyer flasks.Using pipets. transfer S, 10. 15.20. and 25
mL of MOlybdenumSolution A (1 mL 0.2 mg Md) to the
""
flasks. Add 30 mL of dissolving solution and heat until
dissolution is complete,
198.1.2 Increase the temperature and evaporate to HC04
fumes. Coo~ ac1dSO mL otwater and 10 mL of H2S04 (1 +
I). Heat to boiling and cool in a water bath.
198.1.3 Transfer to a SOO-ruL volumetric flask. dilute to
volume. ane! mix. Proceed u directed in 198.3.
198.2 Reagenl Blank Solulion-TransferO.3 g ofiton to a
2S0-mL Erlenmeyer fluk. Add 300 mL of dmolving solu-
tion and heat until di5S01uuon is complete. Proceed as
directed in 198.1.2. 198.1.3,and 198.3.
198.3 Color .Development-Using a pipet. tninsfcr 25 mL
or Iron Solution Band 25 mL of the calibration solution to a
250-mL separatory funneL Add in order, mixing for 15 s
after each addition, 15 mL of NaSCN solution, 15 mL of
SnCI2 solution, and 100 mL of butyl acetate m.ea.sured with a
pipet. Stopper and shake vigorously for 2 min. Allow the
phases to separate, remove the stopper, dnUn oft'. and discard
the aqueous phase. Add to the funnel 50 mL of H2S04 (I +
6), 5 mL of NaSCN solution, and S mL of SnC12 solution.
Replace the stopper and shake vigorously for 2 ",in. Allow
the phases to separate, remove the stopper. drain olf, and
discarci the aqueous phue. Drain enough oftbe butyl acetate
20
 16: 17
330 643 9076 P.05
AST" E353 93 II 0759510 D~~~6bb fbU..
4t E 353
layer through a tUnnel cODWnins a dry filter paper to fiUan T.A8L! 11 St8t11t1c8llnfllflft8tJDIJ-Malybdenll'"
absorpnon "11. (See Note 34.) Malytldenum
Rt Y R ~7
J98.4 Reference Sohaioll-Butyl acetate. Ttal /viA Faunci
~.
(".. E 173"'1 (1'.. IE173"1
'
198.5 Photomelry:
198.5.1 Multiple Cell Photometer-Measure the reagent 1. No. 1. E 850 0.012 0.001 0.005
2. StllnlBSS stB8l13Cr (IIIBS 73c 0.089 0.010 0.010
blank (which includes the cell comction) using absorption 0.011110040)

cells with a (.em light path and a light band centered at 3. No.3.E350 O.'Ia 0.0'2 0.03
approximately 475 om. UsinS the tcst cell, ta1ce the photo- 4. S.1ea8 11M! 'BCr.'ONI (NBS 0.432 0.010 0.0t?
10'41 0.426 Mo)
metric readinp of the calibration solutions. 5. No.4, E350 0.51 0.02 . 0.06
198.S.2 Single Cell Photorrr"er- Transfer a suitable par- 6. SlIiIIl8BII ItBel1I1Cr.15Ni iTi '-34 0.032 O.09Z
110n of \be reference solution to an absorption ceU with a INSS 348 1.~ Mo)
l-cm light path and adjUSt the photometer to the initial .. TN. lest was peffcntl8d in ICCCttIanc;ewIIh 11\81980 .,1IlIIon 01 PnIctic8
setting. usins a light band centered at approximately 475 nm. E 173.
While maintaining this acljustment, take the photometric
readings of the calibration solutions and the reagent blank. appropriate aliquot to a 25()..mL separatory funnel con-
198.6 Calibratioll Curve-Plot the net pbotometric read. taining the appropriate amount of iron solution for the
ings of the calibration solutions qainst milligrams of molyb- specified aliQuot. Add in order, mixing for 15 s after each
denum per 100 mL of butyl acetate. addition. IS mL of NaSCN solution. 15 mL of SnCl4
solution, and. measured with a pipet, the amount of butyl
199. Procedure acetate specifiedh, \he aliqllOtpic1e. Stopper the separatory
199.1 Test Solution; funnel and ~haJce vigorou!ly for 2 min. Allow the phases to
199.1.1 Transfer a 0.3-g sample, weighed to the nearest separate, remove the stopper, drain ofT, and discard the
milligram to a 250.mL Erlenmeyer flask. Add 30 mL of aqueous phase. Add \0 the funnel SOmL oCl-hSO.. (1 + 6). 5
dissolving acid. Add HCl. or MCO:!. or combinations of the nil. of NIiSCN solution, and 5 mL of SnO:z solution. Re-
tWo with or without ~eraJ drops of lIF, and heat until place the stopper and sbake vigorously 2 min. AUOW the
dissolution is complete. phases to separate, drain otT,and discard the aqueous phase.
199.1.2 Increase the temperature and heat to HCl04 DraiD enough of the solvent layer through. I funnel contain-
fulneS. Continue fuming until chroznium, if present, is ing a dry filter paper to fill ao absorption cell. (See Note 34.)
oxidized and tbe white HCI04 nunes are present only in the 199.4 Rt/erence Solution-Butyl acetate.
neck of the Dask.. Add, witb care, 1.0 to 1.5 mL of HCJ, 199.5 Photometry-Take tbe photometric reading of the
aUowin; it to drain down the side of the Oask. (f' thm is test solution and of the reagent blank solution as directed in
evidence of the volatilization of cluomyl chloride, make 199.S.
repeated additions of HCI, followed by fuming after eath
addition. unul most of the cbromiuln has beeo volatiliied. 200. CalculatioR
COn11nl1efuming the solution ulla1 the volume has been 200.1 Convert the Det photometric readin& of the test
reduced to about IS mL. Cool, add SO mL of water and 70 solution to milligrams of molybdenum in the final $Olution
mL of H;tSO.. (1 + I), beat to boilinc. and cool in a water by means of tbe appropriate calibration curve. Cak\11ate the
bath. If the solution is not clear, filter tbe solution through an percentage of molybdenum as follows;
II-cm (me filter paper, coUectins the filtrate in a volumetric Molybdcnum.~ = «o4)/IB x \0» (16)
Ruk that provides for dilution in accordance with the luide
given in 199.1.3. Wash the paper wi\h five 5.mL portions of where:
HzSO.. (1 + 99) collectin, these in the same volumetric flask. A molybdenum. mg, found in 25. SO. or 100 mL, as
"" appropriate of butyl acetate. and 'the aliquot volume
Proceed as directed in 199.3. Jfthe solution is clear, proceed
to 199.1.3. used, and
199.1.3 Transfer to a volumetric flask that provides for B $ample, to represented in 25. 50, or 100 mL. as
"" appropriate, of butyl acetate and the aliquot used
dilution in accordance with the foUowing aliquot guide,
dilute to volume and mix. (see atiqllot guide 199.1.3).
Weishtof 201. PrecJsioa and Bias'"
Sampleia
AliqUOL IroJ\ Butyl Pinal Silty' 201.1 Precision-Nine laboratoriescooperatedin testing
Dilulion, VoluJ\\e. Solulion A=tIIe. Ace1aIe this method and obtained the precision data summarized in
Mol~um.~ m~ mL B.mL ~L Selution.I
Table 17. This method is identical with mQ)ybdenum in
0.01 \oO.OS 200 100 None 2S 0.15 accordance with Test Methods E 350, E 351, and E 352. The
O.OStD O.$S SOO SO None SO 0.03
0.40 \0 1..sO 500 2s 2S 100 0.015 fact that the precision for different materials is comparable
suggeslJlthallhe precisiODof these methods are tbe same.
Proceed as directed in 199.]. 20 1.2 Bias-The a~ of a method can be judged by
199.2 Reagent 814nk Solurion- Transfer 0.3 g of iron to B companng the certified value of a standard wi\h the arith-
2S0.mL Erlenmeyer flask. Add 30 mL of dissolving solution metic average oftbe test data.
and heat until dissol\,nion is c;omplete. Proceed as direeted in
199.1.2, 199.1.3, and 199.3, using the same dilution and
aliquots used for the test solution. ,~
SUppCI"i"1dam II a1l8ila~ I'rom ASn,t HwIq\l8&ft. Requc8I RJI.:ECi3-
199.3 Color DI\'eJopmellt-Using a pipet. transfer the IOU

21

ociety t.OT TestiDg A: Materials

 ASTn
CHROMIUM BY mE ATOMIC ABSORPnON
102. Scope
202.1 This method covers the determination
mium in CODcentrations from 0.006 to 1.00 %.
103. Summary of Method
203.1 The sample is dissolved in mineral acids and the
residue fused, dissolved, and combined wnl1 the soluble por-
tion. The sample lOJunon is aspirated into a nitrous oxide-
acetylen~ flame of an atomic absorption spectrophotometer.
Spectral enerzy at approximately 3579 A from a chromium
bollow-cathode lamp is passed through the flame, aDd the
absorbance is measured. The spectrOphotometer is calibrated
with solutions of known chromium concentrations.
204. Concenh'8rion .Range
204.1 The recommended concentration range is from
0.001 to 0.015 mg of chromium per miUilitre of solution.
205. Interferences
205.1 Because iron acts as a d~ressant, the calibration
solutions must contain approximately the same concentra-
tion oi iron as the \est solutions.
106. ApparafUS
206.1 A.lomic Absorption Spectrophotometer, capable of
resolvinl the 3S79 A line, equipped with a chromium
hollow-c:athode lamp, and a laminar now nitrous oxide
burner. The performance of 111ewuument must be ~ch
that it meel:$ the limi!! defined io 208.4. If your instrument
does not meet this criteria, you CiIlDOt expect to obtain tbe
,
precision and accuracy stated in this method.
107. lleaeenCi
207.1 Chromium Standard SolUtion (1 mL
Cr)-Transfer 2.8290 g of potassium wchromate (~Ci10?)
(NDS 136 or equivalent) to an SOO-mL borosilicate beaker,
add 500 mL of water, and mix. When dissolu1ion is
complete, add S mL of H1804 and, while stirring, add 10 mL
of H~~t (30 %). Heal at near boilin,g fot S min to remo~e
excess "201' Cool, transfer the solution to a l-L volumetnc
flask. dilute to volume, Ind mix. Using a pip:!t" uanaf~r 20
mL to a 200-mL volumetric: .flask, dilute to volume, and mix.
207.2 Iron,l! Low Chmmium-Cr <0.0001 ~.
207.3 PtJlQSsium Carbonate Solution (50 slL)-Dissolve
SO g of potassium carbonalC (K2COj) in water aDd djlute to
1 L. Store the solution in a polyethylene bottle.
208. Preparac10n ot Calibration Curves
208.1 Calibration Solutions for Concentrations 0.005 to
0.10 %-To e&eh of seven 2S0.mL borosilicatc beakcrs.
transfer 1.0 g of low chromhun iron weighed to the nearest I
mg. Add to each beaker 20 mL ofHO and 10 mL ofHNO,
and heat gently until dissolu.tiQD is complete. Evaporate to
dryness on a hot plat; and cool. Add 10 mL of HCI and
warm to dissolve wts. Dilute to about SOmL and ~nsfer to
IOO-mL volumetric flasks. Add 10 mL ofK2CO) solution to
'. JOlmsolt-Mallhq spon,e il'Oft or
s* ltan hu be<:n round >..hable for Lili.
PU/IIOSI:.
Copyright by lbe AmeriCflD Society For Testing II: Materials
Fri Sep 18 13:50:16 1998
E353 93 II O?S~S10 C5~~ab; ~I' .. 330 643 9076 P.06
Q~ E 353
METHOD each of? flasks. Using pipets, transfer 1, 3, S, 7, 10, and IS
mL of chromium standard solution to each flask respec-
tively. Designate the seventh flask as zero chromium concen-
of chro- tration. Dilute to volume and mix.
208.2 Calibralicn Solution for COl1cenrrarions 0.10 to
1.00 %- Transfer 2 & of low cbromium iron wciahed to the
nearest I mg to a 2S0-mL borosilicate beaker. Add 20 mL of
HCI and 10 mL of HNO). Warm as necessary to dissolve the
sample. Evaporate just to dryness on a hot plate and cool.
Add 20 mL of HO and warm to dissolve salts. Dilute to
about 100 mL and add ZOmL ofK2CO) solution. Transfer a
200-mL volumetric flask, dilute to yolutne, and mix..
Transfer lo..mL aliquots to each o(seven lOO-mL volumetric
flasks and add 9 mL of HCI to each nask. Using pipets,
transfer 1, 3. S, 7, 10, and IS mL of chromium standard
solution to each flask respectively. Designate the seventh
flask as zero chromium concenuation. Dilute to volume and
mix.
208.3 Photometry:
208.3.1 With the chromium hollow-cathode lamp in po-
sition, enersized and stabilized, adjust the wavelength to
maximize the energy response of the 3579 A line. The
wavelcDgU1 setting in the vicinity or 4289 A may be wed
provided that the instnlment meets the penormance require-
mcnts.
208.3.2 Li&htthe burner, allow it to thenna1ly equilibrate,
and aciju$t the insuument to zero while aspiratins water.
Aspirate the chromium soluuon with the highest concentra.
lion rrom the seriesprepared as directed in 208.1. and adjust
the burner, nitcous oxide, and fuel pressureJ and flow rates to
obtain maxirnum response. Whenever one or more oithese
parameters are changed, recaJibration is required.
208.3.3 Aspirate the chromium solutions used in 208.3.2
to assure that tbe absomance reading is repeatable. Jle~rd 6
readings, and calculate tbe standard deviation. s, of the
IS 0.1 mg
readings as follows:
s
""
(.4 - 8) x 0.40 (17)
wbere:
It = tbe highest of 6 values found, ano
B ... tbe lowest of the 6 values found'"
20R.J.4 Using water as a reference solution. and begin-
ning with the solution to which no addition of chromiuJJl
was made ia ~08.1 and 208.2, aspirate each cll1ibration
solution in tUrD and record its absorbance. If the value {or
the solution with tbe highest conccntR.ticn diffeIS from the
average of 6 values caJculated in 208.3.3 by more than twice
the standard deviation. or by more than 0.01 multiplied by
the average ot the 6 values, whicbever is greatet, repeat the
measurement. If a problem is indicated, determine the cause,
correct it, and repeat the steps in 208.3.1 through 208.3.4.
208.3.5 Proceed immediately as directed in Section 209.
208.4 Calibration for Concentrations from 0.005 to
0.10 %-Plot the net absorbance values against milligrams
of chromium per millilitre on rectangular coordinat~ paper.
Calculate the deviation from linearity of the ;urve as follows:
Deviation Crom linearity = (C- D)/E (Ii)
t.The wlue 0.40, which il IIICdLO&tlm.le \he _.."I dcviacion fro'" 'lie
ohls valvO!, IIIU publlslle4 by 011011. W. J. and MIlliCY. F.l.. J""odua/tm
"''''Ie
10 Srall.llltJI/.A.""/~I. McGl1Iw.HilI. N~ Yl)rIt. NY. I PS7. p, 404. Table Sit (I).
22
 Ib: 18
330 643 9076 P.07
ASTn E353 ~3 .. 075'5LD DS25&bA 533 ..
ct e S53

where: TABlE 1. Saatltl1callnfOflMlion-Cl\fOmium

C absorbance value for 0.015 mg CrImI..
...
CIImmIIIm R-.I ..... ly
A-oduc:itllli
D absorbance value for 0.010 mg Cr/mL, and Test MaIIll18t Faund . -'J
""absorbance value for 0.005 m.8Cr/111L.
E ""' S
(A.. E
173'" IRa- E 173"1

If the cakulated value is less than 0.60, make the proper ,. No.1.e 35D 0.00&3 0.0014 0.003
2. Nil.3. Ii3St 0.&5' 0.026 0.062
adjustments of instrument or bollow cathode lamp, and. 3. No.Ii.E3&0 0..8&1 0.038 0.093
repeat the calibration. The absorbaDce value for C must be ..
TIlls 181\ WB8 ptrfClnned 1/1acrzrd8/Ic:8 wllh \he 1980 VtIrIion of Practice
0.200 or higher. e 173.
208.S Calibration for Concentrt2tionJ from 0.010 to
1.00 %-Proceed as directed in 208.4. the standard deviation, s, found in 208.3.3, or more than
0.01 multiplied by the average of 6 values used to calculate s,
209. Procedure whichever is gester, determine the cause and repeat the
209.1 Test Solution: calibration and aspiration of tost sol\1tions.
209 .1.1 Select and weigh a sample in accordance with the
followina: 210. CaJadation
Tolmnct DiIIJtion HCltD ~ Final 210.1 Convert the absorbance of the test solution and the
Chfo- Sample in Sample "Ru Di. Aliq,.ol AcIded Dilu- reasent blaak to milligrams olchromium per millilitre of the
mium. Wci8/lt, Weil!lL solUtion. Rcquired. to "II. UOR.
fmal test solution by means of the appropriate calibration
8 III' all. mL ~UOI.ml mL
cu.rvc.Calculale tbe percen. chromium as follows:
"
O.OOS.o.IO
O.ID-l.00
I
I
0.10
0.10
100
100
0
10 ,
o 100
100
Cbromlum,,,- (A-B) xC
. (19)
Transfer it to a 2So.mL borosilicate beaker. W x 10
209. L2 Add 20 mL HC!. 10 mL HN03, and S drops or where:
HF. Heat to dissolve. Remove from the hot plate and dilu.le A - chromium, mg, per mL of final test solution.
to approximately so mL. Add a small amount of filter pulp B "'" chromium, ms. per mL of final reagent blank solu-
and tilter the solution through ll-cm fine filter ""per into a tion,
2S0.mL boro$ilicate beaker. Wash the paper 5 times with
e "" final volume of test solution, and
HCI (I + 99) and n:suve the f1luatc.
209.1.3 Transfer the paper ane! cODtentsto a t:llatinum
w -
weight of Slsnple. in a. in final volume of test
solution.
crucible. Dry on a hot plate. eel traDSferto a mume fUMace
that is less than 400.C. Gradual~ heat to 600.C and hold at 211. Precision and Biasi.,.
this ternpenture for 1 h. Cool, add 0.5 iii of K2C03 and 211.1 Preci6ion-Nine laboB\Oriescooperatedin testing
carefully fuse ovcr a free flame until a clear melt is obtained this method and obtained the precisioDdata summarized in
(see Note 3~). Cool and add IS mL of water. Add HC! Table 18.
dropwise until reaction ceues. Add S drops aCHCI in excess 211.2 Bias-The accuracy can be inferred from the data
and warm on a bot plate, if necessary to obtain a clear in Table 18 by comparing the certified values for chromium
solution. with the averagevalue obtained by using this method.
NOTE 3S-Fusion of \be residue i&maclc in order LOinclude in the CHROMIUM BV TIlE PEROXYDISULFATE
sample solution any chromium thaI mi&lll exist in the sample in an add OXiDA.TlDN- TITRATION MEDlOD
ilUOhablll form.
~12. Scope
209.1.4 Transfer this £OluUod to the filtrate from 209.1.2
and evaporate just to dryness. Add JO mL HCI and warm to 212.1 This method covers tbe detennination of chro-
dissolve salts. Transfer quantitauvely to a IOO-mL mium in conccntmions from 0.10 to 35.00 %.
vohunctric 11uk, dilute to volume. and mix. For samples
with expected chromium. concentrations less than 0.10 ~ 113. Summary of Metbod
proceed as directed in 209.3. For sample!l with expected 213.1 Chromium in an acid sotulion or the sample is
chromium concentration &J"C&terthan 0.10 %, tIa11Sf'erby cxidized to the hexavalent state with ammonium pcroxy-
pipet 10 mL to a lOO-mL volumetric flask, add 9 mL oCHO, disulfate in the pre5ence of s.ilver nitrate catalyst. The sample
dilute to volume, and mix. is then titrated with excess ferrous ammonium sulfate to
209.2 Prepare for each co~ntration range a reagent reduce chromium and the excess back-titrated with either
bJank by treating the same amount of all reagents as directed potassium permanganate or potassium dichromate de-
in 209.1.1 through 209.1.4, includins the low chromium pending upon the presence or absence of vanadium.
iron. Use reagents from the same tots for blank and test Nan; 36--lA the dichromatetitration, the vanadium is not oxi~ed
solutions. alon8 with the excelS feITOU5ions and. thuefore, the voIlime of
209.3 Photometry-Using water as a reference solution, clichtomare added ROa:U tile:lolal ohuaatlium and chromium ud !be
aspjrate and record the absorbance of the calibration. teSt, calc:ula1e4 value for pcI'CeIIt Cr Is hiab. In the I!CJ1D&qaJ1Itetitration.
the Vrv is oxidized to vy. there)' C:OJDJIeI1SIbnl for mc rcctuc:tiOD of
and reagent blank solutions. After each group of 4 or fewer vaDadilUD by rcmm sull'atc in a PRVious "lID.
test solutions and rcasent blank solutions has beep aspirated,
apply the: teat U$i.ns the standard solution. as directed in
208.3.4, dcpending on the concentration I'!U1g1:. If the value 17Slipponin, dilla In aimlll; traM ASTM Headqll~ Reqllesl !tit:
differs from the average of the 6 values by more than twice EOJ.IOJO.

23

CoPnilht by the American Socicly For TeatiDJI Katerials

rn Sap 16 13:50:23 I1J96 "

ASTft £353 93 II C1SQS1D U~c~Ob'
41f/9
%14. Interferences
.~.
214./ The clements ordinarily prcscnt do not interfere if
~. their <:onc:entrationsare less tban the maximum limits shown
in 1.1.
214.2 Each of the following eJemenu. When present above
the indicated limit imparts color to the solution so that
diphenylamjne sulfonate indicator ca.nnot he used when
KZCr207 is chosen as the back-titrant. The limits are; Dickel
1.300 g, copper 0.260 g, and tungsten 0.005 g. The effects of
the elements are additive. If the numerica..l value of the
followidi expression docs not exceed 1.300. the indicator
may be used:
(2.604 + 0.05B + O.OIC) D (20)
where:
It ... tungsten, %, in the saDipIe,
B .. copper, %, in the sample,
C = nietel, %, in the sample, and
D ;;: sample weight, g.
When the value exceeds 1.300, the end point must be
determined potcntiometrical1y if K2Cr2Oris the back-titrant.
us. Apparatus
215.1 Apparatus/0' PotentiometricTitralions-Appara-
tus No. 3D (Ptactices E 50) with a saturated calomel refer-
ence and platinum indj~tor eleetrOde.
ZJ6. RC"Ients
216.1 Ammonium PCTtJxydisuljatcSolution-Dissolve 15
g of ammonium peroxydisulfate [(NH.c)2Sz0a] in water and
dilute to tOO mL. Do not use solutions that have stood for
more than 24 h.
216.2 Ferrous Ammonium Sulfate. Standard Solution
(0.05 Nand 0,10 H)-Reagent No. S (Practices E 50) but use
20 and 40 g of Fe{NH4h<SO.h' 6H20, res~ctively, instead
of the specified weight. Standarclize the solution as directed
in 217.1, 211.2, or 2J 7.3 depending upon the titration
procedure to be employed. Use only if tbe solution has been
standardized or restandardized within 24 h.
216.3 PotassiumDichromate. Standard SolUlion (O.OS N
and 0.10 H)-Reagent No. 10 (Practices E SO) but
'*
2.4518 and 4.9036 Bofrecrylltallized K2Ct~07 (NBS J36c) or
. equivalent primary standard. gnde. instead of the specified
weight.
216.4 PotQssium permanganate, Solution (25 g,lL)-Dis--
solve 25 g oE rcqent grade KMn04 in 200 mL of water,
dilute to I L. and mix.
216.5 Potassium Pe,manganale Standard Solution (0.05
Nand 0.10 N)-Reagent No. 13(Practices E SO)but use 1.6
and 3.2 I of KMn04' respectively, i1utead of tbe specified
weight. Standardin as directed in 34.2 of Praclices E SObut
use 0.1500 G of sodium oxalate (NBS 4Oh) or equivalent
primal')' Standard grade.
216.6 SilverNUrlJl1! Solwion (8 g/L)-Reagent No. 133
(Practices E SO).
216.7 Sodium Diphenylamine Sulfonate Indicator Solu-
,;QfI (2.0 gfL)-Reagcat No. l21 (Ptacliccs E 50).
216.8 1./0 PhenOonthro/ine Fe"ous Complex Indicator
Solulion (0.025 M)-~t No. 122 (Practices E SO).
Copyrighl by the American Society or Testiug k Halerials
Yri Sep 18 13:50:34 1998
330 643 9076 P.08
~'I ..
E 353
117. Staztdardiza.ion of Ferrous Amdlonium Sulfate Sola-
don
217.1 Against PotaJsium Permanganate Solurton:
211.1.1 Tra1Qfer 180 mL of watcr, 12 mL of H}80.
(1+1), and S mt ofH3PO, into a 50o.mL Erlenmeyer ftask.
Add 20 mL of 0.05 or 0.10 N Fe(NH4MSO.~ with either
0.05 or 0.10 N KMnO. solution (216.5) from a 2S-mL buret
and record the volume to the nearest 0.01 mt. Add 1 to 2-
drops of 1,10 phcnanthroline indicator solu.tion. Using a
25-mL buret, titrate the ferrous ions with O.OS N KMnO.
standard soluuon (216.5) while swirling Ute ftask. As the trod
point is approached. add KMnO. dropwise. Continue until
the pink color changes to clear green and persists for at least
60 s.
217.1.2 Calculate the nonnality of the Fe(NH..MSO.)2
solution as follows:
Nonnality ,., ABIC (21)
where:
A - normality of KMnO. soluuon (216.5),
B - KMnO.. solution,mL. and
C Fe(NH.h<SO.h solution, mL,
2!""7.2 Again.rt PotQSsium DichrQmate Solullon Using
Diphenylamine Su(fonaze End Point:
217.2.1 Transfer 180 mL of water, 12 roL of H2S04
(1+1). and 5 mL ofH3PO. into a SOO-mL Erlenmeyer flask.
A.dd20 mL orO.05 or 0.1 0 N Fc(NH.hCSO.)2 (216.2) from a
25-mL buret and record the volume to the nc:arest 0.01 mL.
Add 2 drops of diphenylamine sulfonate indicator solution,
Using a 25-mL buret, tiuate the ferrous ions with either 0.0.5
or 0.10 N KzCr20, solutioD. while swirling the Oask. As the
end point i$ approached. add the K2Cr;Z07 titrant dropwise.
Continue until a blue <:olor appears and penists for at least
30 s. 'Record the buret reacimg ~ the nearest 0.01 mL. Refill
thc burets, add the same volume ofFc(NH.MSO')2 solution
as before and again titrate: witb either 0.05 or 0.10 N
KzCr:O, solution to the blue cnd point. Subtract this volume
of ~Cr2o, solution from the volume recorded for the first
tittation and record the difference as the indica~or blank.
217.2.2 Calc~late the normality of the Fe(NH')2(SO.h
solution as follows:
Normality .. (O_OSor 0.10 (A - B»/C (22)
where:
A = O.OS or 0.10 N K2Cr20, solution, mL. used in the first
titration.
8 ... raL equivalent to the indicator blank, and
C .. Fc(NH4MSO..)z solution, mL, used in tbe first
titration.
211.3 Against Potassium Dichromate Using POlenli~
metric End Point:
211.3.1 Using a 2S-mL buret, transfer 20 mt or 0.05 or
0.10 NK2CrZO, solution into a 600-mL beaker. ResCtVCtbe
remaining 0.05 or 0.10 NK1.Cr2,O,solution in the buret for
tbe back-titration. Add 150 mt of water, 10 mL of H:SO.
(1+1), and S mL of H3P04. Inscn the IAturated calomel
reference electrode and the platinum indicator electrode into
the beaker and connect them to the potentiometer apparatUs.
While stirring the solution, add f'e(NH.MS04)2 until the
dichromate ion yel10wcolor disappears and then a sli&ht
exa!SS.Record the volume offhe Fc(NH..h<SO<\)2 soiution lO
the nearest 0.01 mL. Back-titrate with the remaining 0.05 or
24
 330 643 9076 P.09
ASTrt £353 93 II 015'510 DS25B1U ~~~ ..
4t E 353
0.10 N KZCr207solution by adclins the solution in O.1-mL Cover the beaker with a ribbed cover &lass and heat at as to
inacanenta as tile end point is approached. Record the IDOtCuntil the sample is decomposed. Add sgfficjcnt HN03
vol. when equilibrium is reached after each O.1.mL in small increments to oxidize iron. Boil 2 miD to expel
incren\cftt Inspect the cia.. for the maximum voltagecbaogc oxides of njtr08cn. Proceed as directed in 218.41.
per O.l-mL increment. De1em\me the voltage change for the 218.3 Iftbe Blloy does not dissolve in the acids specified in
O.t-mL increments before and after 1his maximum chanse. 218.2, add amounts of HCJ or HN03. or mixtures acd
Determine the two differences between the tl\n:e voltage dilutions of these acids or bromine and HCI in a ratio of 1 to
~ eomapondiqlo the volume (0.1-mL) increment 3 plus a few drops ofHF, which ace sufficient to dissolve me
before the maximum. the maximum. and after the max- sample. When dissolution is complete. add 80 mL of H2SO.
ilJ2um. This is a very close approximation of the second (1+5) and S mL of H3PO. and evaporate to light fumes.
derivative ot the volume venus cunse ju voltap curve Rinse the cover walls of tho beaker. Again evaporate to
COItespcnldingto the maximum iaf1ectiOftif this tU1'VC was fUmea and fumc for 1 min. Cool, add 100 m.L of water and
plotted. Sum the two voltaic difl'en:nccs.Determine the rauo beat at 85 to IOO.C unW salu are dissoJved.
of the first of these two ditTercnc:eato the wm aDd multiply 218,4 Dilute the solution to ISO mL, add paper pl.l1p,and
0.1 mL by this ratio to obtain the vol~e to be added to the titter tbroup iJI 11<ID rme paper into a SQO.mL Erlenmeyer
smaller volume betWeen\he tWo incremehw additions that flask or a 600-mL beaker jf the potentiometric timtiDD
the maximum change in.voltage oc:curnd. See the foUowing procedure is to be used. Wash the residue 10 to 12 times witb
example: warm water, and J'eSCJVethe filuate.
v 0IU1118 or 0.0) N 218.5 Transfer tbe paper and residue to a platinum
K~30, Val"" 6VoJ\38I CilfclCTlCe BcI'cm cNcible, cbar the paper, and ignite at 850 to goo'C Cor IS
11_ Ti",at (mL) (-VI (IIIV) ud AI\et MuiIQUI'II
min. Cool. add sufficient H2SO. (1+ 1) to moisten the
20.80 555 residue, and then 3 to S mL ofHF. Evaporate to dtyness and
20.90 510 SO 50
21.00 620 100 20 heat at a sraduaJly iDcreasinglate until H~O.. is tCmoved.
21.10 no 80 Fuse the residue with a minimum amount of either fused
21.20 100 sodium hydrogen ,ulfate (sodium pyrosulfate-NazS107) or
21.30 us powsium pyrosulfate (K~O,). Cool the crucible. place in a
:U.40 '54
2S0-mL beaket. and diMOlve the melt in 20 mL of H2SO,
Maximum voltage change occurred between 21.00 and 21.10 (1+ 10). Remove the Ct\Ic:ible, rinse with water, traDsfer the
mL ofK)Cr20, solution. The changes in voltage were SOmV solation to the reserved filtrate (2J8.4), and dilute to 200
belore the maximum, 100 mV at me maximum. and 80 mY mL.
after the cnaximum. The tWo differences between the max. 218.6 Add S mL of AcNO] solution and 20 mL of
imum correspcmdinS to before and after thc maximum were (NH,h~O, solution. It a beaker is used, cover it with a
SO and 20 mV, respcc;tively. Their sum equals 70 and the ribbed cover gillS&.Boit the solution 8 to 10 min maintaining
mio of the fltSt to the sum equals 50170. Thus 50110 the volume at 200 mL by additions of hot water. If the eclor
multiplied by 0.1 mL must be lJIIded to sml&llcr volume due to pennanganate ions does not develop, or develops but
between tbe tWOincrements where the maximum changc in
does not persist, add 2 drops of KMnO. solution (216.4). 5
voltage oceutted. The end point is 21.07 mL.
mL more of AgN03 soJUtiOIi. and 20 mL more of
211.3.2 CaJc:ulate the nonnality of the Fe(NH.)2(SO~h (NH,)zS20. solution, and boU for an addic.ional 8 to 10 min.
solution as follows:
Add hot water to mainta.1n 1be volume at 200 mL durini tbis
-
Normality 0.05 Dr 0.10 AIB (23)
o~ratioD and the operations that rouow in 218.7.
wh=: 218.7 Reduce tbe permanganatc ions as follows; Add 5
.4.. 0.0501' 0.10 N K2CrZ01solution, mL. and mL of HC (1+3) and continue boilirlg for 10 miD after the
B .. Fe(NH.h(SO.):/ solution. mL. disappearance of pamanganlte color. If the pcnnanpnate
ions have not been completely reduced or if a precipitation
218. Praeedure of Mn02 is present, add 1 mL ofHO (1+3) and boil apin
218.1 Select and weigh a sample jn accordance with the for 10 min. Repeat the addition of HO ane! boiling until all
followin&; manganese is present as colorless manpnous ions. Cool to
Sample Weipl, TaIc~ ilL NormalllY of
room tempe~ture and dilute to 200 mL. If vanadium is
Chromium, & SaIllJlle Wciahl, IJI, 11"1"15 present or its absence has not been contirJnecl. proceed as
0.10 \II 0.50" 3.50 :2.0 0.0) directed in 218.8. Ifvaoadium is absent and the criteria of
Q.40 10 1.00 2.00 1.0 0.0$ 214.2 are met, proceed as directed in 218.9. If vanadium is
0..0 \0 1.60 I.~ 0.5 0.05
1.$0 10 3.50 0.50 0.3 0.05
absent and the criteria of 214.2 are not met, or if
:UO to too D.H 0.1 o.O! potentiometric titration is preferred and vauadium is absent,
..00 to 14.00'" 0.50 0.1 0.10 proceed as directed in 218.10.
13.00 to 20.00'" 0.40 0.1 0.10 218.8 Titration With PotlUS;um Permanganale-Whi1e
11,00 \0 30.00'" US 0.1 0.10
.28.00 \0 33.00" 0.20 0./ 0.10 swirling the ftask, add I to 2 drops of 1,10 phmanthroJine
indicator solution aDd then add sufBclcnt Fc(NH.h(SO.h
.. \M 5G-ftL In&rct:.(or \hiI _Imioa I8I1P .ucad at t"~ 3-mL bums solution to etrcct a change in color rrom clear green to pink.
~il\tIIc~ Add ] to 2 xnL more and record the buret rcaclins to the
Transfer it to a 600-mL beaker. nearest 0.01 mL. UsiD. a 2S.mL bum, back-titrate the
218.2 Add 80 mL otH2SO. (1+5) aDd 5 mL ofHJPO.. excess ferrous jons with O.OSN KMnO. .standard solution.

2S

'opyright by the American Society For Testing It MAtena)!

fri Sep 18 13:50:42 1998
 15:21
330 643 9076 P.W
AST" E353 93 II D7S9~~U U~c~ft,~ UCD ..
4t E 353
Add KMnO. dropwise a5 the end point is a,pproacbed. TABLe 11 Stltlillcllinformation-Chromillm
~
. Continue the titration until the pink color has clumged to Chromium
Repeatability P.eprodUCIllllfly
cleargreenwhich,persis~for 60 s. Recordthe buretreading TeSI M,lIIrtaI FOIInG.
(II" E 17304)
to the nearest 0.01 ml. . (Rt. E 17304)

218.9 Titration with PotarsiUM Di,hr{Jmate to the t. No.2. E 360 0.461 0.015 <I.m
2. No.2. e 351 1.9& 0.10 0.16
Dip/JenY/anlint Sul/onace End Poinl-While swirling the 3. No. a. E31i2 U& 0.18 0.48
flask,add Fc(NH4MSO.)z solution from a 2S.mL buret until 4. Stainless SteBI. 13Cr (NBS 12.87 o.ze 0.28
tbe disappearance or me yellow color. Then add 1 to 2 mL in 1331. 12.890)
5. HIgh AlloyVI/ve Sleet (NeS 21.6~ 0.1& 0.68
excessand record the buret reading to tbe nearest 0.01 mL 346. 21.81 Cr)
Add 2 drops of diphetlylamine S\1lf'onateindicator solu1ion. 6. A28S(NiS 348. 14.64Cr) ".55 0.15 U1
Using another 25-mL butct. back-titrate the CXCC5S
ions with O.OS N KzCr2O, standard solution. Add the
fmous A
E 1'13.
TI'is 11181 wa performecIln eccardanc8 with tilt ,980 venuon of PracIicII

KZCr207soJution dropwise as the end point is approached.

Continue \he titration until a blue color appear.; and persistS Although samplC$ at the lower and midrange of the scope
for at least 30 s. Record the bu~t reading to tbe nearest 0.01 were Dot tested, the precision data for other types of alleys
mL. using the methods indicated in Table 19 should apply.
218.10 Titrtllion with Potassium Dichromate and 220.2 Bias-No information on the accuracy of this
Potentiometric End Point DeteCllon-Srir the sample solu- melhod. is known. The accuracy of thjs method may be
tion in tbe 60Q.mL beaker with a magnetic stimr and illKtt judged. however. by comparing accepted reference values
the saturated calomel reference and. platinum indicator with the correspondioz arithmetic averap obtained by
electrodes. With the electrodCi eonnectcd to the potentiom- interlaboratory testiul (see Table 19).
eter apparatus, add from a 2S-mL buret the Fe{NH,MS04h
solution while stining, until the yellow color disappears. VANADIUM BY THE ATOMrC ABSORPTJON METHOD
Then add I to 2 mL in excess and record the buret reading to
the nearest 0.0J mL. Usina another 2S-mL buret add 0.05 N 221. Scope
K1Cr"O, stqndarcl solution in O.l-mL incrementa recording 221.1 This method coven the detcnuination of vanadium
the voltage after equilibrium for each increment. Icspect the in concentratioDs from 0.006 to 0.15 %.
data for the muimum 'Voltqe change between increments of
$1andard dichromate solution (see 2l7.3). Detennine the 222. Summary of Method
voltage change for the increments before ano after the
maximum change and interpolate the end point to the 222.2 The sample is dissolved in hydrochloric, nitric. and
pe.rchloric acids. An aluminum solution i$ added as a
nearest 0.01 mL as described in 217.3.
spectrochemical buffer. The sample soluuoD is aspirated into
219. CakuJation a nitrous oxide-acetylene flame of an a'&Omic absorption
spectrophotometer. Spectral energy at approximately 3 18.4
219.l If KMn04 was used, ca.lcuJate the percentage of
nm f'rom a vanadium hoUow cathode lamp is passed throUBh
chromium as follows:
Chromium, % ... {(AS - CD»)( 1_733JIE (24)
the flame, and ~CI absorbance is measured. This absorbance
is compared wilh the absorbance of a series of standard
where; calibration iolutions.
A = Fe{NH.chCSO,hsolution, mL.
B nonnaUty of Fe(NH4MSO')2 solution. 123. Concentration Range
""
C .. KMn04 solution used, mL, 223.l The recommended concentration range is 0.002 to
D normality of tbe KMnO, solution, and 0.016 mg vanadium per millilitrc ofselution.
""
E = sample taken, g.
219.2 If K2Cr20, was wed. calculate the pe~ntage of 2%4. Interferences
cbromium as follows:
Chromium, ~ ,.. (AB CD) x 1.733)/£ - (25)
224.1 Iron interferes by acting as a depressant. This
interference is overcome by the addition of aluminum
wbere: chloride. whieh acts as a spectrochemical butTer. Titanium
A IS f"e(NH')2(SO..)2solution. mL, and tungsten interfere wben present in concentrntions
B - nonnality of F~}z(S04h solution, greater than O.S and 1.0 %. respectively.
C =' ~Cr~07 solutioD. mL
E .
D = normality of KzCr:O, solulion. and
sample taken, C.
125. Apparatus
225.1 Atomic Absorption Spearopholometcr. capable of
resolving tbe 318.4 nm line. equipped witb a vanadium
110. Precisiolt and Biu" hollow-cathode lamP. aad a laminar flow Ditrow oxide
burner. The performance of the instrument must be such
220.1 Pret:isjon~Nine laboratories cooperated in testing that it is suitable CorUBeas described in Guide E 1024.
this method and obtained the data summarized in Table 19.
226. Reagepts
Suppottill, Ibla aVlUiahle from ASTM HudqllDf1c". RcqllC:ll ~1:O3. 226.1 Aluminum Chloride SolUtion (1 mL = 20 me
"
1036. '"" AI)-Dissolve 90 g of aluminum chloride (A1CJ3.6 H~O) in

26

Copyright by the Ameriaan Society For Te8tlllf .t ~teriab

Fri Sap 18 13:50:52 1998

ASTM £353 ~3 II D75q5~U u~c~e(~
o e 353
approximalcly 300 mL ot water, add JO mL of HCl, and
dilute to SOOrot.
226.~ ViZlltldiwn, Standard Solution (1 mL 0.2 mg
V)-D1SS01ve 0.200 S of vanadium (purity: 99.9" min-
- as given in Guide E 1024.
imum) in 20 mL of aqua regia (three ~olumes ofRCI \0 one
volume ofHN03). Evaporate to near dtynCS$ and add 10 mL
of HCL Cool, transfer \0 is 1-L volumetric l1ask, dilute to
volume, and miA.
Nare 37-As a'll altemalive to vanadium metal. ammoo.ium
rnttavllnadl11emay be used to prCl)1le rhe StaDdard VlJladium solution.
It is prcgared IS follows: Dry several anms of ammonium mcavatladate
(NH. VO~) minimum purity: 99.9 ", in an air oven at IOS10 IIO'C fot
at Iea5t I b and c:ooIlO mom ~mpcratla/'e in IIdesiccator. Weich O.4~92
I oftbe dried product into &600-mL beaker, add 400 mL Dthot water,
anG acntly simm"" to dissolY&.Coot, tmlSCcr to a l000.mL voilimetric
flask. dilute to volume, ancl mix (I mL = 0.20 nil V).
21'7. Prepantioa of'CaIlbratjoll Curve
227.1 Calibrmion Solutions-To each of five, 2S()..mL
bOfosilica1.ebeaken, add 10 mL of HCl04. Using a
mic.roburet. transfer 0.0, 1.0, 2.0, 4.5, and 8.0 mL or
vanadium stalldard so1ution to each beaker. rcspectively.
Cover willi a watch glass, beat, and evaporate to fumes.
Continuc heating ul1Ulsolutions arc neat dryness (Note 38).
Cool, diS$Olve\he salts wilh 10 mL of HC aDd 20 mL of
water. Filter \brough a medium-porosity fitter paper into a
lQO.mLvolumetric flask, wash weD with warm HO (2 +
100). Cool, add 10 mL of Ala, solution (226.1), dilute U)
volume, and mix.
NOT! 38- The remaininl amount Dr HCIO. must be at a IDinimwn.
227.2 Photometry:
. 227.2. t Witb the vanadium hol1ow-cathode lamp in posi-
tIon, cneraized and stabilized. adjust the wavelength to
maximize the energy response of tbe 3 J8.4 nm line.
221.2.2 LiSht the bumer, allow it to reach thermal eQui-
librium, and adjust the instrument to ~o while aspirating
water. Aspirate the vanadium .solution with the highest
concentration from the series prepared as directed in 227.1,
and adjUit the burner, l1iU'ous oxid.e, and fuel pressures anet
flow rates to obtain maximum response. Whenever one or
more of these parameteB arc changed, reca.tibration is
nccessary.
227.2.3 Aspirate the vanadium solution used in 227.2.2 to
assure that the absorbance reading iI repeatable. Record six
absorbance readings. and calculate the Standard deviations,
where:
oS .
s. of the readinp as follows:
(A - .8)x 0.40 (26)
A = the highesl absorbance of the six values found. and
B ... the lowest absorbance of the six values found.12
227.2.4 Usin.g water as a.~ference. ud begin nine with the
solution to which no addi1.1onof vanadium was made it!
~27.1, aspirate each calibration solution in tum and record
Its absorba.ncc.I.fthe value for the solution with the highest
coDct~traUOndiffm from the average of six values calcu-
lateclIn 227.2.3 by more thaD twice 1be Standard deviation
or by more than 0.01 multiplied by the average of the si~
valves, whichever i$ greater. repeat the measurement. If a
proble~ is indicated. detennioe the cause, take appropriate
corrective me~ures;. and repeat 227.2.J through 227.2.4.
227.2.5 Calibration Curve-Plot the average net
27
Copyright by the American Society For Testiug & )faterial!
Fri Sep 18 13:51:00 t99B
330 643 9076 P.ll
Ib~"
absorbance values apinst millisrams of vanadium per
miUililreon rcclanllular coordinate paper. Test faT linearity
228. Procedure
228.) Test Solution:
228.1.1 Transfer 1.0 g of sample, weighed 10 the nearest 1
mg, to a 2SD-mL borosilicate bea1cer. .
228.1.2 Add 20 mL of RCt, 4 mL of HNO,. and cover
with a cover glass. Heat until dissolution is complete. Add 10
mL of HClO. and evaporate 10 fllmes. Continue heaUP8
l10til solutions are near dryness (Note 38). Cool, dissolve the
salts with 10 mL orHO and 20 mL oCwaler. Filter through
a mcdium.pofosi.ty filter paper into II lQO.mL volumetric
flask. and wash weUwitb warm HCt (2 + 100).Coo), add 10
mL of AlCI) solution (226.1). dilute to volume, and mix.
228.1.3 Prepare a reagent blank by using a 250-mL
borosilicate beaker aDd proceeding as dim;ted in 228.1.2.
Usc reagcrtts rrom the same lots as those used tor the $ample
solution.
228.2 Phorometry-Using water U II reference, aspirate
and record the absorbance of the calibration, &ample, and
re8gCDt blank solutions. After each sroup of four or fewer
samplcs and reagent blank solutions have been aspinted,
apply the test using the standard solution as directed in
2~1.2.4. Ihhe value ditretS from the avCf8&coCthe six values
by more tban twice the staDdard deviation, $, found in
227.2.3. or more than 0.01 multiplied by the avcntge of 5ix
valuCl used to cak;ulate $. whidlcVCf is gR:Ater.determine the
cause and repeat the c;a!.ibratioD,sampJe, and reagent blank
measuremenls.
229. Cah:ulation
229.1 Canven the absorbance oCme sample solution and
the rea&cnt blank to milligrams of vanadium per millilitre of
tbe (mal dilution volume by means of the calibration curve.
Calcula~ the percent vanadiu.m as follows:
- -
Vanadium, % «(A B) x IO)/C (27)
where:
A vanad~\lmper mL of the final sample solution. mg,
B '"
... vanadium per mL of the rU1alreagent blank solution.
mg, and
C ..., weight of sample. g.
230. Precision and Bia5J1
. 230..1 Pr~ision- Twenty-three laboratories participated
In testing this method under the auspices of WCi-9 of ISO
Committee TC 17/SC 1 and obtained the data summarized.
in Table 20. All testing meets the requirements of Practice
E 173.
230.2 Bia.f-No information Ola the accuracy of this
method is known. The aCiCUracy of this method may be
judged, however, by companng accepted reference valuC&
with the corresponding arithmetic avera,ge obtained by
interlaboratory testing.
 330 643 9076 P.12
AST" E3S3 ~3 .. U1~~~~u "....-
~m'I' &: 3 S3

TABLE 20 81.8UaIlcallnrollNltlon-V-,adlvm flask. Add SO ntL of H2S04 (1+3) and dissolve at less than
V8II8dJu'" Repell- ISO.C. Oxidize tbe titanium by addiul HN03 dropwisc
RtptOdlldbUlty
Found. .biII~ E 73")
(.112,1 (Note 39). Cool, dilute to volume: with H2S04 0+9), and
(Alte 113") mix. UsiuS a pipet, uansfer 10 mLto a l()().mL volumetric
$18InIenStMI(JSS 852-7. 0.031 VI "
O.03f 0.003 O.OOS Oask, add 10 mL Qr tartarle acid solution. <1iluteto volume,
No.1. E350 0.107 O.DOS 0.014
No.1. E 361 0.008 0.002 0.003 and mix. Do not use a solution that has stood morc: than one
No.1. U52 0.032 0.002 0.004 day.
No.2. E352 0.1S1 0.007 0.011
Ners 39-AII excess of HN03 ,bowd be avoided. Two to three
"This 1011w.. performod IrI K1OGfc1ar1C18
willi lilt 1980 VII'8ICIII
01 Praet1c8 cir'oPfof HNO] ihould be S\1fficicntto oxidiZl:chc litanium iulfatc
E113, so/unon Ind disctwBcthe blue color.

TOTAL 11TANU.rM BY nil: DlANTlP'YRYLMII.'"l'fiANE %38. PreplU'Sltlon of Calibration Cun'e

SPECt1tOPHaJ'OMETRIC ME'IHOn 238.1 Prepare a new calibration cutve for each new lot of
DAPM.
231. Scope
238.2 CaJibrtUioll Solutions-Using pipets, tramfer O.S I I,
231.1 This method covers the determination of titanium 2,4,6.8, 10. 12, and 14 mL oftit.\nium solution (I mL-
in concen'rations from 0.01 to O.;S %. 0.0 I0 mg Ii) to SO-mL volumetric Oasks.
232. Summary of Method NotE 40- Take spectrophotomcmc~np of the ca1ibrationiOIu-
lions contail\lns 0..5, /. Z. 4, allc16 mL ottitanium sohmoll usinlll..cm
232.J Dissolution of the sample is roUowed. by miuctiOI1 liJbt path. Use . l-i:mlight path ror the rcmainint solUtions.
and complexation of interfering elementS. The titanium 4,4'
dianripyrylmcthaDe complex is formed and determined 238.3 R(/'erence Solution-Water.
spectTophotorne1ricaJly. The spcccrophototnetr1c measure. 238.4 Reagent BJanJc-Transfer 10 mL or water to a
S().mL vo1umelric flask and proceed as directed in 238.5.
ment is made at approximately 390 om.
238.5 Color Developmenl,'
233. Concentration Range 138.5.1 Add 3.0 mL of(HCll+l) and 5 mL of ascorbic
acid solution azut allow to stand for 10 min. Add 10 mL of
233.1 The recommended concentration range is 0.006 to DAPM solution. dilute to vQlume witb water, mix, and allow
0.140 mg of titanium per SO IDL of solution. A 2-em cell
should be used for concencratioD$of 0.006 to 0.070 mg of the solution to stand for alleast 90 min.
238.6 Spectrophotometry:
tilanium. A l-em cell should be used tor concentrations of 238.6.1 Multiple-Cell SpectrophOlometer-Measure the
0.070 to 0.140 mg of titanium.
cell correction using absorption cells with either a l-c:m 5gbt
L 234. Stability of Color
234.1 The color takes 90 rnin \0 devclop at ambient
palh or Ii 2-cm light path and a light band centered at
approximately 390 nm. Using the test cen, take; the
spectroptlotometric readinp of \be calibration solutions und
lemperature and then is stable for up to 12 h. the reagent blank $Oluuons versus the reference solution.
235. Interferences 238.6.2 Single-Cell Speclropholometer- Transfer II. suit-
able portion of the reference solution to Ill:)absorption cell
235.1 The elements ordinarily present do not interfere if with a 1- or 2-cm light path and adjust tbe spectrophotom-
their concenuations are under the maximum limits shown in eter using a light band centered at approximately 390 nm.
1.1. Wbile m.uutaining this adjustment, talce the spectrophoto.
metric readinss of the calibration so1utions and the: reagent
236. Appll.l'Atu5 blank solul.ions.
236.1 Glasswt2fe-To prevent contamination of the 238.7 CQlibration Cul'tle-Subtract the reagent blank
sample, aU glassware must be cleaned with hot HCI (1+1) reading from each of the calibration solution readinp. Plot
before use. the blank-coaected spectrophotometric readW&5 of the cali-
bntion solutions apinst mUJigramsof titanium per SOmL
131. ReaaCDts oCsolution.Prepare separate curves fot I aDd Z-cmlipt path
237.1 Ascorbic Acid So/ulion (100 g,tL)-Dissolve 25 g of cells.
ascorbic acid in water and dilute to 250 mL. Prepare as
needcc1. 239. Procedure
237.2 Diantipyry/meth4ne (DUM) (~O g{L)-Dissolve 5 239.1 TestSolution:
8 of 4,4'-diantipyrytmethane monobydrate (C13H2AN40:HzO) 239.1.1 Select a. sample weight in accordance with the
in HCI 0+9) and dilute to 250 mL with the dUute following:
hydrochloric acid. Prepare as needed. Sample T oJarallce in filial AliQIIOI
237.3 PottUJ;um Hydrogen Sulfate. Fused (a mixture of TiWUllm. WeiiJIl, Sample Weis/lt, Volumc. Volumc. Cell
K~207 and KHS04). 96 I ML MI- Siu. CIII
237.4 Tartaric Acid Sohutoll (100 KlL}-Dissolve SOg of "" I 100 10.1)0
MI 10 0.07 1.00 %
tanaric acid in water and dilute to 500 mL. 0.07100.14 1.00 I 100 10.00 I
231.$ Titanium Su(fare SrandtUd
mg 11)- Transfer 0.1000 &of titaa.ium
Solution (1 mL- 0.010
metal (purity: 99.9 %
0.14 tel 0.35 0.40 0.4 100 10.00 I
Transfer it to . 2So-mL beaker.
minimum) weigbed to withiD ::t:O.2mg to a l-L volumetric 239.1.2 Add 20 mL of HCJ and bring to boil. Remove

28

Copyngl1tby the Americ.llnSociety tor Tcstioc It

Fri Sap 18 13:51:11 1998
 .
330 643 9076 P.13
AST" £353 1:1;1_ U'/'!''1~j,U U,!IC~:aO tu.. _
E353
from hot plate and add 5 mL of HNOs. Sample should TABLE 21 SlaIi8tlCat IIIfonn8tIon- TItanIum
diuolve withQut any additiDnal heat. After sample bas R8p8IIaty. ~udDMY.
dissoJved. evaporate the solution to dryness. Teat Mllertll "::"
,,' sill" E 173.) S \R.,E173")
NOTE41-"Ihe UICof a eoane screen or ].mm (lJt.in.) wire, or 1. \..Ow Alloy 0.282 0.0097 0.0228
triaft8la 00 tbe hOl plate, perIIIib more rapid evaporation 1WitholatUte (N6S 170., 0.281 Ti)
daDSeror spaueriq. Z. Cut Iron 0.008 0.00111 0.0037
(Nil 12211,0.007 TI)
Cool, acid S mL of BO to the glass-covered beaker and 3. 11II1 FInIIOe lion 0.33 0.OH8 0.0188
INH 11 0.32 11)
d4s0lvc tbe iron salts at 90 to l00'C and then add S mL of 4. HW1 Alloy 0.078 0..0022 0.Q065
water. INSS 344. 0.016 TI)
239.1.3 f"llter through an ll~em medium-porosity filter S. SpeeIIIty SIBeI 0.20 O.ons. 0.0143
paper containing paper pulp jnto a l00-mL volumetric nask INBS 11541. 0.21 T1)

and rinse lhe beaker and filter paper three times each with "TNt tall w.. IIIriormeO In IccordInGe whit the 1&80 v"slon of PfsCliCO
hot water. Remove the iron salta by washinl the paper with EI73.
10 mL of Het (1+1) anei hot water. Volume in the flask at
this point showd not exceed 70 mL 241. Precision and Bills
2,41.1 Preci$icm-Ei&ht laboratorie$ cooperated in testing
Non 42-lr more than 2 ml or uanssten [s prescnt in aliquot
volume. remove soluble portioo or sample from undar nicer t\nmelllZld this method and obtained data summarized in Table ~1.
wash paper$ several lima: witb N~OH (1 + I). DtsI:ar4 wiUbinp. 241.2 Bias-No information on the accuracy of this
method i3 knowu. The bias of this method may be judged by
239.1.4 Tnmsfer the paper to a platinUD1crucible, dry the comparing acc:cpted rcCercnce values with the corresponding
paper and residlaC.,and men beat in a m.ufIlefurnace at about aritbmetic average obtained by interlaboratory 1eSting.
700'C until the carbon is removed. Cool, and add a few
drops OrH~4 (1+1) followeeiby 2 mL orHF. Evaporate to MOLVBDENl1MBY 11IE ION EXCHANGE-
dT)'11e5S,and then heat at a graduaUy increasing rate until the S HYDJtOXYQUlNQLlNEGRAVlMETAlC MEntOD
H2S04 is removed. Cool, add 2 I of fused potassium 141. Scope
pyrosulflte, fuse over a gas burner and.heat u.nilla clear melt
is obtained. Add 10mL oftanaric acid 5OIuLion10Ibe cooled Z42.1 This method coven the determination of molyb-
melt. heat at 90 to lOO.C,and when the melt is Qissolved, denum in concentrations from 1.5 to 7.0 95.
add aIm solution to the reserved tiltn1te in the volumetric
nask (239.1.3). Dilute 10 volume. and mix. 243. Swsunal')' of Method
239.1.5 Using a pipet. Il'BD:1fcta lo-mL portion to a 243.1 Molybdenum is separated from intcJfering elements
SO-mLvolumetric 11ukAndtreat as directed in 238.5.1 wine on an anion-cxchlQ1go resin column using a sequence or
I mL ofHCI (1+1). hydrofluoric: acid + hydrochloric acid (HF + HCI) eluent
239.2 Sample Bfonk Solution-Using a pipet, transfer a solutions. The isolated mOlybdenum is precipitated with
second 100mL portioD of the test solution to a SO.mL a.hydroxyquinoline and wei&bed .. the anhydrous complex.
volumetric flask aDdtreat as directed in 239.1.5 and 238.5.1.
omitting the addition of DAPM. 244. Interferences
239.3 kag"" Bltl111cSolurion-Carry a rea~nt blank 244.1 All interfering elements which are normally present
through tI1e entire procedure \l$iJ)Sthe same amounts of aU arc removed by the aIIion cxchaagc separation.
reaaentS witb the sample omitted (239.1.1 through 239.1.5).
239.4 Reference Solutions-Water and the sample blank 145. AIIPlll'8hJS
solution, as described in 239.S. 245.1 Ion ExcluUlge Column. PolystJlr(!1Ie,I. approxi.
239.5 Spectrophotometry- Take the spectrophotometric mately 400 nun long and 2S mm in inside diameter. tbe
reading of the reagent blank solution venus water and of the bottom IAl'Credto a 2-mm bore outlet, fitted with a b05ecock
test solution versus the sample blank solution, as ~ in or stopcock to control the liquid now. AU parts of the
238.6. apparatus must be col1StNCtcd of Hf-resistant plastic. such
as polytettaf1uoroetbyleae. polyethylene, or po1y(vinyl chlo-
ric1e)(Note 43).:0
140. CaJc:uJation
NOTE43--The ioll cxehallF «:0.1,,= system muSt be c:arduJIy
240.1 Convert the spectrophotometric rwJing ot the teSl IWCnIbiadInd dzccked to avoid possible.\akqc of 80luuClDICQt1taiaiD,
so!ution ~o m.iJ1igams ot titanium by meam of the appro- HF.
pnate calibratIOn curve. Calculate the percentage oCtitaniwn
as fonows: 246. .aleots
TitaDium, - (,4 -lJ)/(C)( 100))( 100 (28) 246,1 A.mmo1Jium Chloride Solution (240 &lL)-Dissolvc
" 240 8 or ammonium chloride (NH...O) iu 800 mL of water.
where:
A IlK tilani\lm found. mg. in the final color deVtlopment Warm to room tempenm~re,dilute to I L, and mix.
solution. 246.2 A.mmonium Fluoride (NH.F).
B = ti~um found.,mg, in tbe reogent blank.
C ... ongmal sample weight, .. as determined in 2)9.1.1. I. Columnl ttOlft LcdOllI . Co.. Iftc~ Tcaacek. NJ. I18vcbeen Couold
...i"'~
atiafactOf)'.

29

pyright by the 4menC4ll

Fri Sep 18 13:51:18 1998
 16:24
ASTM £353 -'3 .
lit E 353
246.3 Ammonium Oxalale ~OCOCOONH..H~O).
.~ 246.4 EDT A. Solution (10 g/L)-DissoJve 10 I or EDT A-
disodium salt in water. Dilute to 1 L and mix,
246.5 Eluent Solutio7lS-Scc Not~ 44.
Nan 44: Warllils--HF causes ~OU$' bwm wllit:h MaY !lOt be
immediately painflJl; teac! th~ paf3lI'aph &aboutHF in lite Safety
PrecautiOJ\ssection or Practices E so.
246.5.J Hydrofluoric Acid/Hydrochloric Acid/Water
(4+1+9S)-To 800 mL of water in a I-L polyethylene
gr,iduate<icylinder, add 40 mL of HF atad 10 ntL of HQj
dilute to I L and mix. Store in an HF-resis1antplastic bottle.
246.5.2 Hydrofluoric ACid/Hydrochloric A.cid/Waler
(1+5+4)-To 300 mL of water in a l-L polyethylene
graduated cylinder, add 100 mL afHF and 500 mt aFRO;
dilute to I L and mix. Store in an HF-msistant plastic boule.
246.5.3 Hydrofluoric ACid/Hydrochloric Acid/Water
(20+2S+S5)--Ta 500 mL of watCl iD a I-L polyethylene
graduated cylinder, add 200 mL HF and 250 mL HCli diMe
to I L and mix. Store in an HF.l'e$istaDtplastic boule.
246.5.4 Hydrofluoric Acid/Ammonium Chloride/Water
(4+60+36)-To 600 mL of ammonium chloride solution
(240 stL) in a l-L polyethylene graduated cylinder, add 40
mL Hf; dilute to I L and mix. Stare in an HF-resistant
plastic boule. (This solution is 14,4 % in ~CJ on a
weight/volume basis.)
246.5.5 Ammonium Fluoride/Ammonium Chloride Solu.
tion- To 600 mL ofammonium chloride solution (240 aiL)
in a l-L polyethylene graduated cylinder, add 41 lofNH.f.
Add water to the 900 mL mark and stir to dissolve.Dilute to
1 L and mix. With na11'ow-rangepH paper. verify that the
pH is betWeen5.6 and 5.8. Irit is above this range, adjust the
/". solution with dropwise additions of HF; if it is below this
ranse, adjuSt the solution with dropwise additions of
NH40H. Store in an HF-resistant plastic bottle. (This
solution is 14.4 ~ in NH.CI and 4.1 % in NH.F on a
weight/voI\lmebasis.)
246.6 a-Hydroxyquinoline Solution (30 g/L)-Dissolve 30
g of a-hydroxyquinoline in 120 mL of glacial acetic acid
(CH3COOH). Cautiously add warer, with stirring to a total
solution volume of 600 mL. Wann to 40°C, Add NH.OH
( 1+ 1)dropwise with stirrins until a slight permane11tprecip.
itate is formed. CarefuUYad.dglacial CH3COOH with stirring
until tbe precipitate first dissolves. Dilute to 1 L.
246.7 lon-Exchange Resin:
246.7.1 Use an anion-w:hange fesin of the alkyJ Q.uater-
nary ammoniulIl type (chloride fonn) consistins of .spherical
beads having a cross-1inka&eof 8 % and of 200 to 400
nominal U.S. mC$hsize.zl To remove those beads greater
than about 180 J.Lmin diameter, as well as the very smaU
diameter beads..treat the resin ASfoUO'II/S: 'emnsfer a supply
of the resin to a beaker, cover with water. and aDowat least
30 rom for the beads to undergo maximum swellins. Place a
No. 80 (180aJ.1m)screen, 150 mm in diameter, over a 2-L
beaker. Prepare a thin uuny of the resin and pour it iDtothe
screcm.Wash the fine beads through the screen wins a small
stream of water. Discard the beads retained on the screen
periodically to avoid undue cloggingof the openings. When
)' AOI.X8. 200-400 mc:sh. d\Ioridc C-. ...hKh i. avaiJabiD ftom Bioobd
Laboratories, Ricltnulu. CA. Iw bcCIIround alisllClory.
A.
Copyright by the American Socicty For Testing 6: Ma .
fri Sep 16 13:51:28 1998
330 643 9076 P.14
O?S'S:LO DS2S&?.!a"':J _
the bulle of the resin has settled in the 2-L beaker, decant the
water and tnu2sfer approximately 100 mL of resin to a
400-rnL beaker. Add 200 roL of HO (1+19) and stir
vigorously. Allow the IeSin to setdc for 4 U) 6 miD, decant
ISO to 175 mL Qr ~ suspension, .a.c1 dlsca.rd. 'Repeat the
treatment with HCt (1+19) twice more, and reserve the
coarse resin for the column preparation.
246.7.2 Prepare the column IS foUews: PIa" a 10 to
20-mm layer of poly(vinyl chloride) plastic fiberU in the
bottom ot the column, and add a sufficient amount of the
prepared resin to fill the column to a heiAbt of approximately
ISO to J7S mm. P1ac;ea 20~aun layer ofpoly(vinyl cbloride)
plastic fiber on the top of the resin sudace to protect it from
being carried into suspension wbcta the solutions arc added.
Add 100 to 125 mL otaci (3+1) to the ~l\lmn. When tne
solution level is S to 10 mOl above the tOp of the rC$in bed
add 100 mL of HCI (1+9) to tho column. Repeat this cycle
twice more and finally wasn tbe resin bed with 200 Jl\L HCl
(1+3) turninS oache stopcock when the solution level is 10
to 20 mm above the top of the resin bed.
246.8 Sodium Hydroxide Solution (! 00 g/L)-Dissolve
100 g of sodium bydroxide (NaOH) iD about 100 mt of
water. When dissolution is complete. cool. and dilute to I L.
Store in a plastic bot1.l.e.
246.9 Sodium Hydroxide Solution (10 8IL)-DiS$Olve 10
S of NaOIi in abou, 100 mL ofwater. Cool and dilute to 1 L.
Store in a plastic bottle.
247. Procedure
247.1 Transfer I g ofsamp1e weished to the nearest 0.1
mg to a 2.00-mLpolytctratluoroetbylenc beaker !narked at
the 100-mL level 00 the outsider. Add 10 mL of Hf and
cover with a polytetraOuoroethylene watchglass. Warm the
solution with low heat and cautiouslyadd HNO) in l-mL
increments aUowingthe reaction to subside betWeen addi-
tioQ$. Higb chromium samples may also require cautious
dropwise additions of RCl. When dissolutiODis complete,
cool the beaker, remove the cover with platinum..\ippcd
toogs and cautiously rinse it i~to the solution with water.
247.2 Over a steambath or other Jow temperature ar-
ransement evaporate the solution to dryness. Cool, wash
down the &idesof tbe beaker with HO (I + 1) ancl again
eVBpotateto dryness over low beat. Cool. add 5 mL Hf and
25 mL water. Warm over low heat unlil aUsalts are dissolved
(Note 45). Cool to room 1emperatuTeand dilute to JOOmL
with 'Water.
Non 45-11 may be Dcccs.saryCOadd additional willer aDd to stic
tAubously with a potycenfJuoroethylellc nimBi rod to completely
dissolve lit wu.
247.3 Drain the solution in the ion exchange column by
passin, 100 mL orlIF/HCtlwater(4+1+9S) throuzh it at a
rat~of approximately2 mL/min. AUowthe solution to drain
10 the top of the resin bed. Collect the cffiuent in a plastic
beaker and discard it.
247,4 Plate an 800-mL plastic beaker under the column.
PIIice a small plastic funnel bolding a high-porosity hard-
surface filter paper in the top or the column. Eusure that an
U Dynel p\a8Jjc _I ~vailablo fioOMUaiOn Carbiclc COtp.. Chemical Divilion.
Ter.liJc Fibora DcIIIU'\ftIcal, Need)wD ticit'llt, MA. bu bccII found I81iar.C\Ory.
30
 16:25
ASTn £3S~ ~3
air seal doc$ not form between the funnel and tbe column.
Cautiously filter 1he sample solution onto tbe column.
AdjuSt the eft1uent llow to about 2 mL/miD. lUnse the
beaker with HFJHO/water (4+1+95) tnlnsfecring the
wuhinas to the paper. Cautiously police the beaker with a
polytetrat1uoroethylene policemaD. if n~. and rinse
onto tbe paper with HFIHC1Iwater (4+1+95). Wash the
paper well with HF'/HO/water (4+1+95). Cautiously re-
move and discard paper (Note 46).
Non 46-If insoluble molybdenum c:ompa\lncb ate suspected
Down to be 1X"csent. bUt the Bow rrom tbe c:olual whm the: wa.shini of
tbe paper is complete. Clilutiolllly 1nI'dsfer thc paper to a platinum
crucible and ipiU: at 500'C (JIGhial\er) in a mumc: r\lmace. Cool i1l II
desic:Qlor. add I . anhydrous ~\Im carbonate powdu (N~C03) and
fuse oYCfa bum". Cool, add 20 mL or wafer anci bcat la dissolve the
meh. CatauUy Kiditt with dropwia additions or RCI (1+4) IIntil
effi=rvcscenceccaxs plus 10 drops excess. EY!\parate 10 dryness, cool.
WI 20 mL HFIHO/_rcr (4...'.95), heat to diIoSOlvc,cool, and transfcr
thi$ !oJulion to Ibe CD'umn. RQumc Ihe 2 mUmin Row from lhe
column.
247.5 Continuetoadd HF/HCVwatcr(4+11-95) unti1650
mL bave been collected in \he BOO-mL plastic beaker (Note
47). Drain solution to the top of the resin bed. Cautiously
discard this solution.
Non 47-Thk amltion conwftS aJl tbe iron. chromium.
CDbalt. a1vminum. ca&:lPCJ',aad martpnlCSe.
247.6 Place an 800-mL plastic beaker under the column
and elute 500 mL of HF/HCltwater 0+5+4) al a:tate of 2
ml.Jmin. Drain solutiou to the top of the resin bed.
Cautiously discard this SOlUtioa (No~ 48).
Non 48- ThIs solQtio~contains all the t\lqstM, titanium, zirco-
nium, IUId hafDilim.
330 643 9076 P.15
.. D7~~~~U
4mtJ E 353
NOTe 51: Warallll-EDSlUC that the app!ie4 lempennure d0C5 nOt
ex~ the $O~IIJ point of po'~lIrO!llbylc~.
247.12 CoOlto room temperature, dilute to about 30 mL
with water, add 5 mL ofHNO) and 5 mL ofHCJ. Coverand
beat for J0 min.
247.13 Dilute to 100 mL. Heat to boiling and while hot,
caU1iousJ)'add NaOH solution (100 &lL)until litmus paper
moistenedwiththe solutionjust turns bluc,tben add 10 mL
excess. Boil tOt 1 min. If a precipiute u prescnt, filtcr
ar
througb high porosity, surface hardened filter paper and
wash paper thoroughly with wann NaOH solution (10 8IL).
Discard paper. Uno precipitate is present, proceed directly to
241.14.
247.14 AcljliSt the volume of (be solution or IiItrate
obtained in 247.13 to about 200 mL. Add 10 mL of EDTA
solution (10 g,lL) and 3 g of ammonium oxalate. Warm
gently to obtain a clear solution and cool to room temp~l1t-
ture. Adjust the pH to 4.0 using a pH meter and dropwise
additions of HCI (1+ 1) and NaOH solution (to aiL).
247.IS Heat tbe solution to boilinc. remove from heat
and slowly add 20 mL of 8-hydroxyquinoline solution (30
g/L) wlUlesdninS. Heat at just below the boiling point for 10
miD.slininl occasionally.
Dickel,
2.47.16 F'1I\erthrough a tared mcdi.um-poro$i.tyfritted
Blassfiltering crucible usiDs ,ende suction. W4t$hthe con-
tents of the beaku into the filtering Cl'UcibJewith hot water
and wash the precipitaw with additiol1llJbot water Cora
toW of about J00 mL.
247.17 Dry the precipitate in a drying oven set at J2S.C
Corat least 4 h. Cool the filtering crucible Corat least 2 h in a
desiccator and weigb.

247.7 Place aa 8OD-mL polyrcuat1uoroethylene beaker 248. Calculation

under the column and chate the molybdenum with 500 mL 248.1 Calculate the percenlage of molybdenum .s foJ-
of HFIHO/warer (20+251"55) at a.rate of 2 mLtmin. Drain lows:
solution to the top ofthe resin bed. Proceed with this eluent
solution as desaibed in 247.11.
Molybdenum. ~ . (IA - B) X 23.0SJIC (29)
247.8 Place an 800-mL plastic:beaker under the column wbere:
and elute 300 mL of HFINH.CI/water (4+60+36) at a rate ..4 - wei&ht of crucible plus precipitate, in g,
of 2 mL/min. Drain solution to the top of the resin bed. B weightof cnJcible.in &.and
""
CautiOtWydiscard this solution (Note 49). C sample weisht, in g.
'"
NOTE 49- Tbi5 5OIution camain5 aI1lhc niobium. 249. PredsioD and Biu
247.9 Place an 800-mL plasUc beaker under the column 249.1 PreciJion-8cvcn laboratoriC$ cooperated in tC$ung
and elute 3.s0 mL of NH.F/NH.C .solution at a rate of 2 this method and obtained the data summarized in Table 22.
mL/min. Drain solution to the top of the resin bed. As indicated, no data are presenUy available to determine the
Cautiously discard this solutio%! (Nore SO). precision of this method. However, tbis method i£ identic:a1
Non 50-This 1OI~lionIIOIIWn$ IIllhe lanwum_ to the ion-elchangc-8-hydroxyquinoline &ravimetric proce-
dure in Test Methods E 351. E 352, and E 354. This fact
247.10 Plac.: an BOO-mLplas1ic beaker under tbe colul2U1
sugaests that the precision for this method is the same. While
and clute 100 mL of w.ter. then 100 rnL of HCI (1.3),
stopping tbe ilow when the liquid level is 10 to 20 mm above the testing range exceeds the upper limit of the Scope, the
data for Ten Material 3 were included to illllStrate the
the resin bed. Cautiously disc;atd the solution. The column is
now ready to be stored for future use or to be preconditioned
for another sample (247.3). TABU! 22 SIaU,tJGII,nfonaation-MolylKlenum Ion Exchlnge-
8-HydroQQellnolln8 Gl'llv/meltle MelJlad
247.11 To the eluent containing the molybdenum (Crom
247.7) cautiously add 15 mL of HzSO. 0+1) and evaporate T881MI III M01yOCIeftum Rlpllletliliev Repl'~
Found.S (R,. e t7SA) IRa.Ei173")
to lipt fumes on a sanclbath or other carefully controlled ,. No.10US,
heat source (see Note S1). Cool and cautiously riuse into a '.48 0.070 O.oSG
2. No.2. 1354 3.92 0.219 0.250
400-mL borosilicate &lass beaker. Heat to low volume (about
10 mL), cool, add 2 mL of HNO). and evaporate to strong
fumes of SO). e 173.
.
3. No.3. E362
TIll. _t was ~
8.85
In ~
0.180 0.188
wI\II\lie 1880 VtnIcIn01,.,aeu,;

31

tOP1" Y tile Amc:ricIIl1 :i'ocie ¥

Yri Sep 18 13:51 :37 1998
 330 643 9076 P.16
ASTM E~S3 ~3 II D?S~S1D U~~~ei' ~~a -
. E 353
ruggedness oftbe method's precision at levels near the upper 250. Keywords
'''--limit of the Scope. 250.1 combustion analysis: gravimetric; induction fur-
249.2 Buu--No data are presently available to deiennine nace; infrcued absorption; total carbon
the accuJaCY of this method.

TIle Am8r1C811S«;Mfy tor 1u11i1tl8lld 14t11.8I1M , 110pGII/JoII 'elpect/nf III. vaUgtfy of tIf/hl. ..,f/1811 {II cannllCllon

willi lilY II.",1rI8IIUotI8dIn 111II.~, I.I4aII r1Ilit" .1.IIIdItrJ '''Y 1M''''''

IIIIptfI4Iy I4Vlced /lilt det8r/IJI1IaIIO01 lilt v.RdIty Of/lilY aell
."
~ .It. aIId 'M nJlt of lIIIr/trr1ettlttlrrJllUl:h rlfIIt.. If' ItIIlrfly Ihrtlrt1'ItfIfIUPOIIII&II/ry.

"Ihi8"wild g filbJlICtt4 1'1\I111IoII.81'1,/ImI 011'/fit ~/ble flCMlCtl_1ItBB IIId 11I11I1 be ffVItIwBdCWfIYDVt ,.,. 8/ld
111101 tithlf ,~ OfwII/'ItIf_ '1_ C0lMl8ll111' II1JIrrrilrlllllrtler 'or fW/IIOIIof tJtlt flfllltlald /!I tor IrldlrlollallllllMlrdl
"'''811.
1M.1IouId be 811111 to AS7M HMtI..,,,,,. '1011ICOIMII/II. 11II1I f8C8Ir8 etrI/IIII CCI/J8/atf111D1r II I fIlMing'" 1M t8JIOfI/Ilbl.
lr/CIttIieMCGfIImMN.rrftk:h ~ ma1 """,d. /I youlH/ ",., 'fOIl' _,. hllVt fIOInJC8/II8IJ. lilt h..mo 'fOIl.-111 /IIIkB yQJI'
1'1_ MOwrr lei U/8 ASTM /:cmmIII8e Stttttdlfd,. 1918 Race SI., PltlJadtlph/8, PA 111103.
'"

Copyright by the AmeriCllJ1 SocieLy For lie Haterials

hi Sep 18 13~l:4? 1998

TOTAL P.16

~'