An American National Standard

Designation: D 2896 – 03

Designation: 276/95

Standard Test Method for

Base Number of Petroleum Products by Potentiometric
1

Perchloric Acid Titration

This standard is issued under the fixed designation D 2896; the number immediately following the designation indicates the year of 
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
cript epsilon (e) indicates an editorial change since the last revision or reapproval.
superscript
supers

This standard has been approved for use by agencies of the Department of Defense.

1. Scope
Scope*
* bility of regulatory limitations prior to use. For specific hazard
1.1 This tes
testt met
method
hod cov
covers
ers the det
determ
ermina
inatio
tion
n of bas
basic
ic statements, see Section 7, Section 10, and X2.2 .
constituents in petroleum products by titration with perchloric
2. Referenced Documents
acid in glacial acetic acid.
1.2 Proced
Procedure
uress A and B use dif differ
ferent
ent tit
titrat
ration
ion sol
solven
ventt 2.1   ASTM Standards:   2
volumes and sample weights. D 1193
1193 Specification for Reagent Water
Water

NOTE  1—A round robin on a series of new and used oils and additive 3. Terminology
concentrates has shown that the two procedures give statistically equiva-
lent results
results.. 3.1  Definitions of Terms Specific to This Standard:
3.1.1   base
base numbe r —the
number — the quaquanti
ntity
ty of per
perchl
chlori
oricc aci
acid
d ex-
1.3 Appen
Appendixdix X2 provides the use of an alte
alternati
rnative
ve solvent pressed
pressed in term
termss of the equiv
equivalen
alentt numb
number
er of mill
milligra
igrams
ms of 
system which eliminates the use of chlorobenzene in this test potass
potassium
ium hydroxid
hydroxidee tha
thatt are required
required to tittitrat
ratee 1 g of the
method. The use of the alternative solvent gives statistically sample
sam ple dis
dissol
solved
ved in the spespecifi
cified
ed sol
solven
ventt to a welwell-
l-defi
defined
ned
equivalent results; however, the precision is worse. Paragraph inflection point as specified in this test method.
X2.5.5 provides guidance when comparing results using the
two different solvents. 4. Summ
Summary
ary of Test
Test Method
1.4 The constituent
constituentss that may be considered
considered to have basic 4.1 The samsample
ple is dis
dissol
solved
ved in an essessent
ential
ially
ly anh
anhydr
ydrous
ous
character
chara cteristi
istics
cs incl
include
ude org
organic
anic and inor
inorganic
ganic bases
bases,, amin
amino
o mixture of chlorobenzene and glacial acetic acid and titrated
compounds, salts of weak acids (soaps), basic salts of polya- with a solution of perchloric acid in glacial acetic acid using
cidic bases, and salts of heavy metals. potentiom
pote ntiometri
etricc titr
titrimet
imeter
er.. A glass indi
indicatin
cating
g elec
electrod
trodee and a
NOTE   2—This test method is applicable
applicable to both fresh oils and used oils calomel reference electrode are used, the latter being connected
as described in Sections 16, 17, and 19 and Appendix X1. with the sample solution by means of a salt bridge. The meter
readings are plotted against the respective volumes of titrating
1.5 This test method
method can be used to deter
determine
mine base number
number
solution, and the end point is taken at the inflection in the
>300 mg KOH/g. However, the precision statement in Section resulting curve.
19 has been obtained only on base number #300 mg KOH/g.
4.2 Procedure A uses 120 mL of of titration solvent. Procedure
Procedure
1.6   This standar
standard d doe
doess not purport
purport to add
addre
ress
ss all of the
B us
uses
es 60 mL of ti titr
trat
atio
ion
n so
solv
lven
ent.t. In ad
addi
diti
tion
on,, th
thee tw
two
o
safe
safety
ty co
conc
ncer
erns
ns,, if an
anyy, as
asso
soci
ciat
ated
ed wit
with
h its us
use.
e. It is th
thee
procedures use different equations for the calculation of appro-
responsibility of the user of this standard to establish appro-
priate sample weights. Since many portions of the test method
 priate safety and health practices and determine the applica-
are identical for Procedures A and B, only the unique sections
will be described separately for the two versions of the test
1
Thiss test method
Thi method is und
underer the jurisdicti
jurisdiction
on of ASTM Committee
Committee D02 on
method.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.06
D02.0 6 on Analysis of Lubri
Lubricants.
cants.
2
Current edition approved Nov. 1, 2003. Published December 2003. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1970. Last previous edition approved in 2001 as D 2896–01 1. e
contact ASTM Customer Service at service@
service@astm.o rg. For   Annual Book of ASTM 
astm.org.
This test method has been appro
approved
ved by the sponsoring
sponsoring committees and accepted Standards volume
Standards  volume information, refer to the standard’s Document Summary page on
by the cooperating societies in accordance with established procedures. the ASTM website
website..

*A Summary of Changes section appears at the end of this standard.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 

D 2896 – 03
4.3 Occas
Occasiona
ionally
lly certain
certain used oils give no infle
inflection
ction in the all reagents shall conform to the specifications of the Commit-
forward titration mode, in which case a back titration modifi- tee on Analytical Reagents of the American Chemical Society,
cation with sodium acetate titrant is employed. where such specifications are available. 3 Other grades may be
used,
use d, pro
provid
vided
ed it is firs
firstt asc
ascert
ertain
ained
ed tha
thatt the reagent
reagent is of 
5. Signi
Significanc
ficancee and Use
sufficiently high purity to permit its use without lessening the
5.1 New and use usedd pet
petrol
roleum
eum pro
produc
ducts
ts can con
contai
tain
n bas
basic
ic accuracy of the determination.
constituents that are present as additives. The relative amounts 7.2  Purity of Water —Unless
—Unless otherwise indicated, references
of these materials can be determined by titration with acids. to water shall be understood to mean reagent water as defined
The base number is a measure of the amount of basic substance by Type III of Specification D 1193.
in the
th
someti
som e mes
oil,
oi
etimesl, use
alwa
always
d ys
used as un
unde
a der
r th
the
e e co
measur
measure cond
ofndit
itio
ions
nsant
lubric
lub of deg
ricant thee radati
th
degradtest
test.
. on
ationIt in
is 7.3  Acetic Acid , glacial (Warning
(Warning—Toxic
—Toxic and irritant).
7.4   Acetic Anhydride   (Warning —Toxic and irritant).
Warning—Toxic
service; however, any condemning limits must be empirically 7.5 Chlor
Chlorobenz
obenzene (Warning—Toxic
ene (Warning —Toxic and irritant).
established. 7.6   Pe
Perrch
chlo
lori
ricc Ac
Acid
id,, StStan
anda
darrd SoSolu
luti
tion
on in Ac Acet
etic
ic
6. Appar
Apparatus
atus  Acid   (0.1  N ) (Warning
Warning—P —Pow ower
erfu
full ox
oxid
idan
antt wh
when
en dr
dry y or
heated
heated.. Gre
Greatat car
caree sho
should
uld be tak
taken
en to avo
avoidid con
contac
tactt wit
with
h
6.1   Potentiometric Titrimeters, eith
either
er auto
automati
maticc reco
recording
rding
organic matter under conditions that may result in subsequent
or manual.
drying or heating, and spills should be washed immediately
6.2   Glass Electrode, pH 0 to 11, general-purpose type.
and
and th
thor
orou
oughghly
ly wi
with
th wa
wateter)
r)—M
—Mixix 8.
8.5
5 mL of 70 to 72 %
6.3  Reference Electrode, sleeve-type saturated calomel elec-
perchloric acid (HClO4, 70 to 72 %) (or 10.2 mL of 60 to 62 %
trode with a nonaqueous salt bridge as described in Section 10.
HClO4  solution) with 500 mL of glacial acetic and 30 mL (or
NOTE   3—Some reference electrodes with fritted or fiber diaphragms 35 mL if the 60 to 62 % HClO 4   solution is used) of acetic
and some combin
combined
ed glass plus reference electrodes
electrodes systems are comme
commer-
r- anhydride. Dilute to 1 L with glacial acetic acid. Allow the
cially available,
available, such as the single-rod glass plus silver/
silver/silver
silver chloride solution to stand for 24 h.
electrode assembly. During the development of this test method, the use of 
electrodes of these types gave problems in some laboratories, but not in NOTE  6—Excess acetic anhydride should be avoided to prevent acety-
others. Accordingly, these electrodes are permitted in this test method, lation of any primary or secondary amines that may be present.
provide
prov ided
d tha
thatt the sodi
sodium
um per
perchlo
chlorat
ratee bri
bridge
dge is use
used;
d; how
howeve
ever,
r, when
7.7   Potassium Hydrogen Phthalate—(KHC8H4O4).
stability or other problems arise with their use, the sleeve-type electrode
should be used.
7.8   Sodium
Sodium PerPerchlor
chlorate
ate Electr olyte—(
Electrolyte Warning—Sodium
—(Warning —Sodium
perc
perchl
hlor
orat
atee is to
toxi
xicc an
andd an ir
irri
rita
tant
nt.. It is al
also
so a po
powe
werf
rful
ul
6.4   Stirrer , eith
either
er mech
mechanic
anicalal or elect
electrica
rical,
l, with variable oxidizing agent when heated. Great care should be taken to
speeds
spee ds anand
d wiwith
th pr
prop
opelelle
lerr or papadd
ddle
le of ch chem
emic
ical
ally
ly in
iner
ertt avoid contact with organic matter under conditions that may
material. When an electrical stirrer is used, it must be grounded result in subsequent drying or heating, and spills should be
so that disconnecting or connecting the power to the motor will washed
washe d imme
immediat
diately
ely and thoro
thoroughl
ughlyy with water.)
water.) Prep
Prepare
are a
not produce a permanent change in meter reading during the saturated solution of sodium perchlorate (NaClO 4) in glacial
course of a titration. A magnetic stirrer with stirring bar can be acetic acid. An excess of undissolved NaClO 4  shall always be
used provided it meets these conditions. present at the bottom of the solution.
6.5   Buret , 10 or 20-mL, graduated in 0.05-mL divisions and 7.9   Titration
Titration Solve nt —Ad
Solvent —Add d one volvolume
ume of gla
glacia
ciall ace
acetic
tic
calibrated
calibrated with an accur acy of   60.0
accuracy 0.02
2 mL, or an aut automa
omatic
tic acid to two volumes of chlorobenzene.
buret of similar accuracy. 7.10   Sodium Carbonate, anhydrous (Na2CO3).
6.6   Titration
Titration Beaker , madmadee of bor borosi
osilic
licate
ate glass or othother
er 7.11   Sodium Acetate Solution, 0.1  N  in acetic acid (for back 
suitable titration beaker, tall form recommended.
6.6.1
6. 6.1 For Pr Proc
oced
edur
uree A, us usee a be
beak
aker
er of 25
250 0 or 30
300 0 mL titration, see Sections 16 and 17)—Dissolve 5.3 g of anhydrous
Na2CO3   in 300 mL of glacial acetic acid. Dilute to 1 L with
capaci
cap acity
ty.. For Procedur
Proceduree B, use a bea beaker
ker of aboabout
ut 150 mL acetic acid after solution is complete.
capacity such that 60 mL of titration solvent will cover the
electrodes. 8. Stand
Standardi
ardizatio
zation
n of Reagents
NOTE  4—Other beakers of suitable size capacity may be used. 8.1   Perchloric
Perchloric Acid Soluti on—The stan
Solution standardi
dardizati
zation
on of the
6.7   Titration
Titration Stand , sui
suitab
table
le to sup
suppor
portt the bea
beaker
ker,, ele
elec-
c- perchloric acid solution (HClO4) differs for the two procedures
trodes, stirrer, and buret. An arrangement that allows for the as follows:
removal of the beaker without disturbing the electrodes, buret, 8.1.1   Procedure A  (120 mL)—Heat a quantity of potassium
and stirrer is desirable. hydrogen phthalate in an oven at 120°C for 2 h and allow it to
cool. Take 0.1 to 0.2 g of the potassium hydrogen phthalate
NOTE   5—Some
5—Some apparatus may be sensitive to interf interferenc
erencee by static weighed to the nearest 0.1 mg and dissolve
dissolve it in 40 mL of warm
electricity, shown by erratic movements of recorder pen or meter indicator,
when the titration assembly (beaker and electrodes) is approached by the
operator. In this case surround the beaker closely with a cylinder of copper
3
gauze that is electrically grounded.  Reagent Chemicals, American Chemical Society Specification
Specificationss, Ame
America
rican
n

Chemical Society, Washington, DC. For suggestions on Standards

the testing for
of reagents not
7. Reage
Reagents
nts and Materials
Materials listed by the American Chemical Society, see   Annual
Society, Laboratory
Chemicals,   BDH Ltd., Poole, Dorset, U.K., and the   United States Pharmacopeia
Chemicals,
7.1   Purity of Reagents—Reagent grade chemicals shall be and National Formulary, 
Formulary,   U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
used in all tests. Unless otherwise indicated, it is intended that MD.

2
 

D 2896 – 03
glacial acetic acid. Add 80 mL of chlorobenzene, cool, and 9. Prep
Preparati
aration
on of Sample
titrate with 0.1   N  HClO
  HClO4   solution, using the electrode system 9.1 It is essential to ensure that the sample
sample is representative
representative
and procedures given in 10.1 to 10.4 and 11.4 to 11.7. Detect since any sediment can be acidic or basic or have adsorbed
the end point by the same procedure used for base number acidic
acid ic or basic material
material from the sampsample.
le. When nece
necessary
ssary,,
determination (see 14.2). Carry out a blank titration on 40 mL samp
sampleless ar
aree wa
warm
rmeded to ai
aid
d mi
mixi
xing
ng.. Us
Used
ed oi
oils
ls sh
shou
ould
ld be
of glacial acetic acid plus 80 mL of chlorobenzene (see 11.8). vigorously shaken to ensure homogeneity before sampling.
8.1.2   Procedure B  (60 mL)—Heat a quantity of potassium
NOTE   8—As
8—As use
used
d oils can cha
change
nge appr
appreci
eciably
ably in stor
storage
age,, sam
samples
ples
hydrogen phthalate in an oven at 120°C for 2 h and allow it to
should be tested as soon as possible after removal from the lubricating
cool. Take 0.05 to 0.1 g of the potassium hydrogen phthalate system and the dates of sampling and testing, if known, should be noted.
weighed to the nearest 0.1 mg and dissolve
dissolve it in 20 mL of warm
glacial acetic acid. Add 40 mL of chlorobenzene, cool, and 10. Prep
Preparati
aration
on of Elec
Electro
trode
de Syst
System
em
titrate with 0.1   N  HClO
  HClO4  solution as described in 8.1.1. Carry 10.1   Preparation
Preparation of Electr odes—Whe
Electrodes —When n the calo
calomel
mel elec-
out a blank titration on 20 mL of glacial acetic acid and 40 mL trode is to be changed from aqueous bridge to nonaqueous,
of chlorobenzene (see 11.8). drain out the aqueous solution, wash out all crystals of KCl
8.1.3 Calculate the normality
normality,,  N A, of the HClO 4  solution as with water,
water, then rinse the outer jacket (salt bridge) several several
follows: times with NaClO4  electrolyte solution. Finally fill the outer
 N A  5  1000W  /[204.23·~V – b !#   (1)  jacket with NaClO4  electrolyte solution up to the filling hole.
When using the slee sleeve-t
ve-type
ype elec
electrode
trode,, caref
carefully
ully remove the
where: ground-glass sleeve and thoroughly wipe both ground surfaces.
W    = potassium
potassium hydro
hydrogen
gen phthal
phthalate,
ate, g,
g, Replace the sleeve loosely and allow a few drops of electrolyte
V    = HClO
HClO4  solution used, mL, and to drain through to flush the ground-glass joint and to wet the
b   = volu
volume
me corresp
correspondin
onding
g to   V   for the blank titration,
titration,
ground
grou nd surfa
surfaces
ces thor
thoroughl
oughly y with electrolyte.
electrolyte. Set the sleev
sleevee
mL.
firml
firmlyy in pl plac
ace,
e, re
refil
filll th
thee ououte
terr ja
jack
cket
et wi
with
th th
thee Na
NaCl ClO
O4
NOTE   7—Beca
7—Becauseuse of the rel
relati
atively
vely lar
large
ge coe
coeffficie
icient
nt of volu
volumet
metric
ric electrol
electrolyte
yte solu
solution,
tion, and rins
rinsee the elect
electrode
rode with chloroben-
chloroben-
expansion of organic liquids, the acetous HClO 4  solution should be used zene
zene.. Wh
Whenen in ususe,
e, ththee elelec
ectr
trol
olyt
ytee le
leve
vell in th
thee ca
calolome
mell
within  6 5°C of the temperature at which it was standardized. If used at a electrode should be kept above that of the liquid in the titration
temperature more than 5°C higher, multiply the volume used by the factor beaker to prevent entry of contaminants into the salt bridge.
1 − (t ·0.001).
·0.001). If used at a temperature more than 5°C lower, multiply by When not in use, fill the calomel electrode with the NaClO 4
the fa
fact
ctor
or 1 + (t ·0.001),
·0.001), where   t is
is the dif
differ
ferenc
encee in deg
degree
reess Cel
Celsius
sius
electrolyte solution, leave the bung in the filling orifice, and
between temperatures of standardization and use and is always positive.
immerse both electrodes in distilled water, keeping the level of 
8.2   Sodium
Sodium Acetat
Acetatee Solutio n—The standardizati
Solution standardization
on of the the electrolyte above that of the distilled water.
sodium acetate solution (Na2CO3) differs for the two proce- 10.2   Testing of Electrodes—Test the meter-electrode com-
dures as follows: bination when first put into use or when new electrodes are
8.2.1   Procedur
Proceduree A   (120
(120 mL)
mL)—Us
—Usee 120 mL of ti titra
tratio
tion
n installed and retest at intervals thereafter as follows:
solvent
solvent and 8.00 mL of 0.1 N HClO
HClO4 solution. Titrate with 0.1  N  10.2.1   Procedure A—Dip the electrodes into a well-stirred
sodium acetate solution, using the electrode system and pro- mixt
mi xtur
uree of 10100
0 mL of gl glac
acia
iall ac
acet
etic
ic ac
acid
id pl
plus
us 0.
0.2
2 g of 
cedure given in 10.1 to 10.4 and 11.4 to 11.7. Detect the end KHC8H4O4  and record the reading given by the meter. Rinse
point by the same procedure as will be used for base number the electrodes with chlorobenzene and immerse in 100 mL of 
determination (see 14.2). Calculate the normality,   N B, of the glacial acetic acid plus 1.5 mL of 0.1  N  HClO   4  solution. The
sodium acetate solution as follows: difference between readings is to be at least 0.3 V.
 N B  5  [ ~8.00 – b ! N A# / G   (2) 10.2.2   Procedure B—Dip the electrodes into a well-stirred
mixt
mi xtur
uree of 60 mL of gl glac
acia
iall ac
acet
etic
ic acacid
id pl
plus
us 0.0.1
1 g of 
where: KHC8H4O4  and record the reading vein by the meter. Rinse the
b   = volume
volume corre
correspond
sponding
ing to   V   for the blank titration, electrodes with chlorobenzene
chlorobenzene and immerse in 50 mL of glacial
 N A   = nor
normal
mality
ity of the
the HClO
HClO4  solution, and acet
ac etic
ic acacid
id pl
plus
us 0.
0.75
75 mL of 0. 0.1
1   N   HClO4   solution.
solution. The
G   = vovolu
lume
me of ststan
anda
dard
rd so
sodi
diumum ac acet
etat
atee us
used
ed in ththee difference between readings is to be at least 0.3 V.
standardization, mL. 10.3   Cleaning
Cleaning of Electr odes—Fol
Electrodes —Followin
lowingg a titr
titratio
ation,
n, first
8.2.2   Procedure B  (60 mL)—Use 60 mL of titration solvent wash
was h the eleelectr
ctrode
odess wit
with
h ti
titra
tratio
tion
n sol
solven
ventt to rem
remove
ove any
and 4.00 mL of 0.1   N  HClO
  HClO4  solution. Titrate as described in adhering oily material from the previous titration. Then wash
8.2.1. Calcu
Calculate
late the norm
normalit
ality
y,   N B, of th
thee so
sodi
dium
um ac
acet
etat
atee the electrodes
electrodes with water to dissodissolve
lve any NaClO4   that may
solution as follows: have formed around the sleeve of the calomel electrode and to
 N B  5  [ ~4.00 – b ! N A# / G   (3) restore the aqueous gel layer of the glass electrode. Rinse again
with the titration solvent. Before starting a series of sample
where: titrations, follow this rinsing procedure, then run one or two
b   = volume
volume corre
correspond
sponding
ing to   V   for the blank titration,
 N A   = nor
normal
mality
ity of the
the HClO
HClO4  solution, and blank tit
blank titrat
ration
ionss on the sol
solven
ventt to con
condit
dition
ion the ele
electr
ctrode
odes.
s.
Repeat the blank titrations if necessary.
G   = volum
volumee of stan
standard
dard acetou
acetouss sodium
sodium acetate
acetate used
used in
10.4   Maintenance of Electrodes—When there is reason to
the standardization, mL.
believe that the glass electrode has become contaminated, it

3
 

D 2896 – 03
( Warning—
can be cleaned by immersion in cold chromic acid (Warning — total change of more than 0.03 V (corresponding to 0.5 pH
Corrosive and carcinogenic) or an alternative non-chromium- scale unit) in the cell potential, add 0.05-mL portions. In the
containing strongly-oxidizing acid cleaning solution for 5 min, interm
intermedi
ediate
ate reg
region
ionss (pl
(plate
ateaus
aus)) whe
where
re 0.1 mL incincrem
rement
entss
follow
followed
ed by tho
thorou
rough
gh wat
water
er was
washin
hing.
g. Aft
After
er thi
thiss cle
cleani
aning
ng change the potential by less than 0.03 V, add large portions
treatment, test the electrode as described in 10.2. The calomel suffficie
suf icient
nt to produ
produce
ce a total potential
potential chang
changee appro
approximat
ximately
ely
electrode can be cleaned by draining and refilling with fresh equal to, but not greater than, 0.03 V. Titrate in this manner
NaClO4  solution. Maintain the electrolyte level in the calomel until the potential changes less than 0.005 V (corresponding to
electrode above that of the liquid in the titration beaker at all 0.1 pH scale unit) per 0.1 mL.
times.
tim es. Do not allow the electrod
electrodes
es to rem
remain
ain immersed
immersed in
NOTE   11—Consider the cell potential constant when it changes less
titration solvent for any appreciable period of time between than 0.005 V/min.
titrat
titration
ions.
s. Whi
While
le the ele
electr
ctrode
odess are not ext
extrem
remely
ely fra
fragil
gile,
e,
handle
han dle the
them
m car
carefu
efully
lly at all tim
times
es and par
partic
ticula
ularly
rly avo
avoid
id 11.6.2   Automatic Recording Titration— Adjust the instru-
scratching the glass electrode. ment in accordance with the manufacturer’s instructions and
set the titration speed at 1.0 mL/min maximum.
11.. Proc
11 Procedur
eduree A (120 mL) 11.7
11.7 On completion
completion of the titration
titration,, remo
remove
ve the beaker and
11.1 Cal
11.1 Calcul
culate
ate the qua
quanti
ntity
ty of sam
sample
ple req
requir
uired
ed fro
from
m its rinse the electrodes and buret tip with titration solvent, then
expected base number,   BN , as follows: with water, then again with titration solvent (see 10.3). Store in
water when not in use (see 10.1).
Approximate weight of sample, g  5  28/expected BN    (4)
11.8
11.8 For each set of samples make a blank titratio titrationn using
NOTE   9—For the back titration procedure (see 16.2), or when analyzing 120 mL of titration solvent. For a manual titration add 0.1   N 
used oils, it may be necessary to use a smaller sample weight. HClO4  solution in 0.05-mL increments, waiting between each
11.1.1 Weigh the sample into the titration beaker, applying addition until a constant cell potential is established. Record
the limits shown as follows. A maximum of 20 g should be meter
met er and bur
buret
et rea
readin
dings
gs aft
after
er eac
eachh inc
increm
rement
ent.. Fol
Follow
low the
taken for analysis. procedure in 11.6.2 for an automatic titration.
Precision of
Sample Weight, g Weighing, g 12. Proc
Procedur
eduree B (60 mL)
10 to 20 0.05 12.1 Cal
12.1 Calcul
culate
ate the qua
quanti
ntity
ty of sam
sample
ple req
requir
uired
ed fro
from
m its
5 to 10 0.02 expected base number as follows:
1 to 5 0.005
0.25 to 1.0 0.001 Approximate weight of sample, g 5  10/expected  BN    (5)
0.1 to 0.25 0.0005
NOTE   12—F
12—Foror th
thee ba
back
ck ti
titra
tratio
tion
n pro
proce
cedur
duree (s
(see
ee 17
17.2
.2)) it ma
may
y be
11.2 Add 120 mL of titr
11.2 titration
ation solvent
solvent to the samp
sample.
le. necessary to use a smaller sample weight.
11.3
11 .3 Pla
Place
ce the beaker
beaker on the titrati
titration
on sta
stand
nd and stir the
solution until the sample is dissolved. 12.1.1 Weigh the sample into the titration beaker, applying
the limits shown as follows. A maximum of 10 g should be
NOTE   10—If solution of the sample proves difficult, dissolve it in 80 taken for analysis.
mL of chlorobenzene in the titration beaker, then add 40 mL of glacial
Precision of
acetic acid. Many used oils contain some solid materials that will not Sample Weight, g Weighing, g
dissolve. This is a frequently observed condition.
5 to 10 0.02
11.4 Prepa
11.4 Prepare
re the elect
electrodes
rodes as directed
directed in 10.1, 10.2, and 1 to 5 0.005
10.3. Position the electrodes in the solution so that they are 0.25 to 1.0 0.001
immersed as far as possible. Continue stirring throughout the 0.1 to 0.25 0.0005
determination at a rate sufficient to produce vigorous agitation NOTE  13—It is especially important for Procedure B that great care be
without
witho ut spatt
spattering
ering and witho
without
ut stir
stirring
ring air into the solu
solution
tion.. exercised
exercised in obta
obtainin
ining
g acc
accura
urate
te wei
weights
ghts par
partic
ticular
ularly
ly for the high bas
basee
Adju
Ad just
st th
thee me
mete
terr so th
that
at it re
read
adss in th
thee up
uppe
perr pa
part
rt of th
thee number samples which require small sample weights.
milliv
mil livolt
olt sca
scale;
le; for exa
exampl
mple,
e, 700 mV mV.. For sim
simple
ple met
meters
ers 12.2 Add 60 mL of titrtitratio
ation
n solvent to the sample.
without this adjustment, it is necessary to incorporate a source 12.3
12. 3 Pla
Place
ce the sample
sample on the titrati
titration
on sta
stand
nd and stir the
of potential in series with the electrode. A 1.5-V dry cell and solution until the sample is dissolved.
potential divider is suitable.
11.5
11. buret with 0.1 N  HClO4  solution and place the
5 Fill the buret NOTE  14—If the solution of the sample proves difficult, dissolve it in 40
mL of chlorobenzene in the titration beaker, then add 20 mL of glacial
buret in position in the titration assembly, taking care that the
acetic acid.
tip is immersed below the level of the surface of the liquid in
the beaker. Record the initial buret and meter (cell potential) 12.4 Prepa
Prepare
re the elec
electrode
trodess as direc
directed
ted in 10.1, 10.2, and
readings. 10.3. Position the electrodes in the solution so that they are
11.6   Titration: immersed as far as possible. Continue stirring throughout the
11.6.1   Manual Titratio n—Ad
itration—Add d sui
suitab
table
le sma
small
ll por
porti
tions
ons of  determination at a rate sufficient to produce vigorous agitation
titrant and, afte
titrant afterr waiti
waiting
ng unti
untill a const
constant
ant potential
potential has been without spat
without spatteri
tering
ng and without stirring air into the solu
solution.
tion.
established (Note 11), record the buret and meter readings. At Adju
Ad just
st th
thee me
mete
terr so th
that
at it re
read
adss in th
thee up
uppe
perr pa
part
rt of th
thee
thee st
th star
artt of th
thee ti
titr
trat
atio
ion
n an
and d in an
anyy su
subs
bseq
eque
uent
nt re
regi
gion
onss milli
millivol
voltt sca
scale;
le; for exa
exampl
mple,
e, 700 mVmV.. For sim
simple
ple met
meters
ers
(inflections) where 0.1 mL of titrant consistently produces a without this adjustment, it may be necessary to incorporate a

4
 

D 2896 – 03
source of potent
potential
ial in series with the electrode.
electrode. A 1.5-V dry cell NOTE  15—Because the base number can vary while the QC sample is
and potential divider is suitable. in storage, when an out-of-control situation arises, the stability of the QC
sample can be a source of the error.
12.5 Fill the
the buret with
with 0.1  N  HClO4  solution and place the
buret in position in the titration assembly, taking care that the
14. Calculation
tip is immersed below the level of the surface of the liquid in
the beaker. Record the initial buret and meter (cell potential) 14.1 For a man
14.1 manual
ual titrati
titration,
on, plot the volumes
volumes of the acid
readings. added against the corresponding meter readings.
12.6   Titration: 14.2 Inte
Interpret
rpret the end point from the graph obtained
obtained from
12.6.1   Manual Ti tration—Add suitable small portions of 
Titration the manual or automatic titration. The end point is the midpoint

titrant and afte

titrant afterr waiti
waitingng unti
untill a const
constant
ant potential
potential has been of the inflection,
concave to convex.that point but
A useful at which the curveguide
not mandatory
mandatory changes from
is that
is the
established (Note 11), record the buret and meter readings. At
thee st
th star
artt of ththee ti
titr
trat
atio
ion
n anandd in an
anyy su
subs
bseq
eque
uent
nt reregi
gion
onss end point is preceded and followed by a deflection of a least 50
(inflections) where 0.1 mL of titrant consistently produces a mV/0.1 mL of titrant.
total change of more than 0.03 V (corresponding to 0.5 pH 14.3 When there
there is no inflection
inflection point or only a very poor
scale unit) in the cell potential, add 0.05-mL portions. In the one, proceed to Section 16 or Section 17 on back titration. The
interm
int ermedi
ediate
ate reg
region
ionss (pl
(plate
ateaus
aus)) whe
where
re 0.1 mL inc increm
rement
entss inflection obtained during back titration preferably is to meet
change the potential by less than 0.03 V, add large portions the criteria described in 14.2.
suffi
suf ficien
cientt to produ
produce ce a tota
totall poten
potential
tial chan
change
ge appr
approxima
oximately
tely 14.4 Calcu
Calculate
late the base number,
number,   BN , as follows:
equal to, but not greater than, 0.03 V. Titrate in this manner  BN , mg KOH/g 5   [~ E  –
KOH/g  –  F ! ·  N A · 56.1]/ S 
S    (6)
until the potential changes less than 0.005 V (corresponding to
0.1 pH scale unit) per 0.1 mL. where:
 E    = H
HCl
ClO
O4   soluti
solution
on use
used
d to tit
titrat
ratee the sample
sample to the
12.6.2   Automatic Recording Titration— Adjust the instru-
inflection point on the titration curve, mL,
ment in accordance with the manufacturer’s instructions and
F    = volu
volume
me corr
correspon
esponding
ding to E  for
 for blank titration at same
set the titration speed at 1.0 mL/min maximum.
potential as sample, mL
12.7theOn
rinse completion
completion
electrodes andofburet
the titr
titratio
tipation,
n, remove
with titrationthe beakerthen
solvent, and  N A   = norm
normalit
ality
y of
of H
HClO
ClO4  solution, and
S    = samp
sample,
le, g.
with water, then again with titration solvent (see 10.3). Store
the electrodes in water when not in use (see 10.1).
15. Repor
Reportt
12.8
12.8 For each
each set of sam
sample
pless make a bla blank
nk on 60 mL of 
titrat
titration
ion sol
solven
vent.
t. For a ma
manua
nuall tit
titrat
ration
ion add 0.1   N   HClO4 15.1 Repor
Reportt the result as follows:
solution in 0.05-mL increments, waiting between each addition Base Number  ~D 28962Procedure A or B! 5  Result (7)
until a constant cell potential is established. Record meter and This report format may not be used when using the alterna-
buret readings after each increment. Follow the procedure in tive solvent described in Appendix X2. Instead, use the format
12.6.2 for an automatic titration. described in X2.4.
13. Qual
Quality
ity Control
Control Checks
16. Back Titration
Titration,, Proc
Procedur
eduree A (120 mL)
13.1 Con
13.1 Confirm
firm the perperfor
forma
mance
nce of the equ
equipm
ipment
ent or the
16.1 Some used oils
oils give no inflection
inflection point or only a very
procedure each day it is in use, by analyzing a quality control
poor one with the test method described in Section 11. When
(QC) sample. It is advisable to analyze additional QC samples
thiss sit
thi situat
uation
ion is enc
encoun
ounter
tered,
ed, the fol
follow
lowing
ing mod
modifie
ified
d tes
testt
as appropriate, such as at the end of a batch of samples or after
a fixed number of samples. Analysis of result(s) from
from these QC method may be use
method used.
d. In thi
thiss mod
modifie
ified
d tes
testt met
method
hod,, exc
excess
ess
standard
standard HClO4   solut
solution
ion is add
added
ed to the sample,
sample, the
thenn the
samples
sampl es can be carr
carried
ied out usin
using
g contr
control techniques.4
ol chart techniques.
excess HClO4  solution is back titrated with standard sodium
When the result of a test on a QC sample exceeds the control
acetate solution.
limits of the laboratory, corrective action such as instrument
16.2 Accur
Accuratel
ately
y weig
weighh the amount of samp
samplele specified in
recalibration, may be required. An ample supply of QC sample
11.1 into the titration beaker. (See Note 16.)
material shall be available for the intended period of use, and
shall be homogeneous and stable under the anticipated storage NOTE   16—The sample size for the back titrati
titration
on modification does not
conditions. If possible, the QC sample shall be representative exceed 5 g. When, with a 5-g sample, no inflection point is found, reduce
the sample size to 3 g and repeat the analysis. Reducing the sample size
of sam
sample
pless typ
typica
ically
lly ana
analyz
lyzed
ed and the aveaverag
ragee val
value
ue and
generally improves the clarity of the inflection point. However, it should
control limits of the QC sample shall be determined prior to be noted that the cooperative work that led to the precision statement (see
monitoring the measurement process. The precision for the QC 19.1) employed a sample size of 5 g maximum.
sample must be compared against that given in the Precision
and Bias section of this test method in order to verify that the 16.3 Disso
Dissolve
lve the sample in 80 mL of chlor
chlorobenz
obenzene
ene and
instrument is functioning correctly. add 40 mL of acetic acid.
16.4 Use a volumetric
volumetric buret or pipet to add accurately
accurately 8.00
mL of sta
standa rd 0.1   N   HClO4   solutio
ndard solution
n to the bea
beaker
ker.. (Th
(Thee
4
standard HClO4  solution must be in excess. If necessary, add
M MNL 7,   Manual
ASTM
AST Manual on Pre
Present
sentatio
ationn of Data Control
Control Chart Analysis
Analysis,,
Section 3: Con
Section Control
trol Cha
Charts
rts for Ind
Indivi
ividua
duals,
ls, 6th ed, ASTM Int Intern
ernatio
ational
nal,, W. more than 8.00 mL and correct accordingly (16.7).)
Conshohocken, PA. 16.5 Stir the contents
contents of the beaker
beaker for 2 min.

5
 

D 2896 – 03
16.6 Titrat
Titratee the unneutralized
unneutralized HClO4  solution with standard 18. Repor
Reportt of Resu
Result
lt for Back Titration
Titration
0.1   N   sodium acetate solution. Carry out the titration in the 18.1 Repor
Reportt the result as follows:
same manner as described in Section 11. For the back titration,
Base Number by Back Titration
the starting point will be in the range from 0 to 100 mV.
~Test Method D 2896 2Proce dure A or B! 5  Result
Procedure
16.7 Instead of weighing out a separate
separate sample and proceed-
proceed-
ing through 16.6, the back titration procedure can be used on a
19. Prec
Precision and Bias   5
ision
sample being titrated as in 11.1 to 11.6.2, provided that the
samp
sample le size did no nott ex
exce
ceed
ed 5 g (s
(see
ee No
Notete 16). When
When it is 19.1   Procedure A (120 mL) :
apparent from the forward titration that a satisfactory inflection 19.1.1 The precision
precision of this test method as determined
determined by

is not present,
present, note the volume
volume of stastanda
ndard
rd HCl
HClOO4  solution statistical
(see Note examination
14 and Note of interlaboratory results is as follows
16):
used,
use d, the
then
n pro
procee
ceed
d wit
with
h 16.
16.6.
6. The stastanda
ndardi
rdizat
zation
ion (8.
(8.2.1
2.1))
should be modified to coincide with the volume of standard 19.1.1.1   Repeatability—Th
—Thee dif
differ
ferenc
encee bet
betwee
weenn two tes
testt
HClO4  solution. results, obtained by the same operator with the same apparatus
16.8 Calc
Calculate
ulate the base number,
number,   BN , as follows: under constant operating conditions on identical test material,
would, in the long run, in the normal and correct operation of 
 BN , mg KOH/g  5   [~G  –  H ! ·  N B· 56.1]/ S 
KOH/g S    (8)
the test method, exceed the following values only in one case
where: in twenty:
G   = volu
volume
me of ststan
anda
dardrd so
sodi
dium
um acacet
etat
atee us
used
ed in th
thee % of Mean
standardization, mL (see 8.2.1 or 8.2.2), All oils with forward titration 3
Used oils requiring back titration 24
 N B   = norm
normalit
ality
y of the sodium
sodium acetate
acetate solution
solution,,
 H    = vo
volu
lume
me of ststan
anda
dardrd so
sodi
dium
um acacet
etat
atee us
used
ed in the
the NOTE  18—Since there were insufficient data from the 1986 cooperative
sample back titration, mL, and study to determine the precision for the back titration procedure for used
S    = wei
weight
ght of sam
sample
ple,, g. oils, the back titratio
titration
n precision data are those obtained in the 1972 study.
A new coo cooper
perati
ative
ve stud
study
y is pla
planned
nned to det
determ
ermine
ine the bac
back
k titr
titrati
ation
on
17. Back Titratio
Titration,
n, Procedure
Procedure B (60 mL) precision
precis ion using modern instrumentation.
instrumentation.

17.1 Some used oils

oils give no inflection
inflection point or only a very 19.1.1.2   Reproducibility—Th
—Thee dif
differ
ferenc
encee bet
betwee
ween
n two
poor one with the test method described in Section 12. When single and independent results obtained by different operators
thiss sit
thi situat
uation
ion is enc
encoun
ounter
tered,
ed, the fol
follow
lowing
ing mod
modifie
ifiedd tes
testt working
worki ng in dif
differe
ferent
nt labo
laborator
ratories
ies on ident
identical
ical test mate
material
rial
method
met hod may be useused.
d. In thi
thiss mod
modifie
ified
d tes
testt me
metho
thod,
d, exc
excess
ess would, in the long run, in the normal and correct operation of 
standard
stand ard HClO4   soluti
solution
on is addadded
ed to the sample,
sample, the
thenn the the test method, exceed the following values only in one case
excess HClO4  solution is back titrated with standard sodium in twenty:
acetate solution. % of Mean
17.2 Accurately weigh the amount specified in 12.1 into into the All oils with forward titration 7
titration beaker (see Note 17). Used oils requiring back titration 32

NOTE   17—The sample

sample size for the back titrati
titration
on modification
modification does not NOTE   19—The ranges
ranges of base number values for which these precision
exceed 2.5 g. When, with a 2.5-g sample, no inflection point is found, values were established are given in Appendix X1.
reduce the sample size to 1.5 g and repeat the analysis. Reducing the 19.1.2   Bias—Th
—Thisis pro
proced
cedure
ure in Test Met
Method
hod D 2896
2896 for
sample size generally improves the clarity of the inflection point.
measuring base numbers has no bias because the base numbers
17.3 Diss
Dissolve
olve the sample in 40 mL chlorobenz
chlorobenzene
ene and add can be defined only in terms of the test method.
20 mL of acetic acid. 19.2  Procedure B (60 mL) :
17.4 Use a volumetric
volumetric buret or pipet to add accurately
accurately 4.00 19.2.1 The precision
precision of this test method as determined
determined by
mL of sta standa
ndardrd 0.1   N   HClO4   solutio
solution
n to the bea
beaker
ker.. (Th
(Thee statistical examination of interlaboratory results is as follows:
standard HClO4  solution must be in excess. If necessary, add (see Note 14 and Note 16):
more than 4.00 mL and correct accordingly (17.7).) 19.2.1.1   Repeatability—Th
—Thee dif
differ
ferenc
encee bet
betwee
weenn two tes
testt
17.5 Stir the contents
contents of the beaker for 2 min. results, obtained by the same operator with the same apparatus
17.6 Titrat
Titratee the unneutralized
unneutralized HClO4  solution with standard under constant operating conditions on identical test material,
0.1   N   sodium acetate solution. Carry out the titration in the would in the long run, in the normal and correct operation of 
same manner as described in Section 12. For the back titration, the test method, exceed the following values only in one case
the starting point will be in the range from 0 to 100 mV. in twenty:
17.7 Instead of weighing out a separate
separate sample and proceed-
proceed- % of Mean
ing through 17.6, the back titration procedure can be used on a All oils with forward titration 5
sample being titrated as in 12.1 to 12.6.2, provided that the
19.2.1.2   Reproducibility—Th
—Thee dif
differ
ferenc
encee bet
betwee
ween
n two
sample size did not exceed 2.5 g (see Note 17). When it is
single and independent results obtained by different operators
apparent from the forward titration that a satisfactory inflection
working
worki ng in dif
differe
ferent
nt labo
laborator
ratories
ies on ident
identical
ical test mate
material
rial
is not present,
present, note the volume
volume of sta
standa
ndard
rd HCl
HClOO4  solution
used, the
used, then
n pro
procee
ceedd wit
with
h 17.
17.6.
6. The sta
standa
ndardi
rdizat
zation
ion (8.
(8.2.2
2.2))
should be modified to coincide with the volume of standard
HClO4  solution used. 5
Supporting
Supporting data have been filed at ASTM International
International Headquarters and may
17.8 Calc
Calculate
ulate the base number
number as descr
described
ibed in 16.8. be obtained by requesting Research Report RR:D02-1011 and RR:D02-1237.

6
 

D 2896 – 03
would, in the long run, in the normal and correct operation of  20. Keyw
Keywords
ords
the test method, exceed the following values only in one case
20.1 bas
20.1 basee num
number
ber;; per
perchl
chlori
oricc aci
acid;
d; pet
petrol
roleum
eum pro
produc
ducts;
ts;
in twenty:
potentiometric titration
% of Mean
All oils with forward titration 7

19.2.2   Bias—Th
—This
is pro
proced
cedure
ure in Test Met
Method
hod D 289
2896
6 for
measuring base numbers has no bias because the base numbers
can be defined only in terms of the test method.

APPENDIXES

(Nonmandatory Information)

X1. TEST COVERAGE

COVERAGE

X1.1 Durin
During
g the development
developmentss of the original
original test method
method used will not introduce serious errors in the precision.
(Proceduree A) and the test method for the reduc
(Procedur reduced
ed titr
titratio
ation
n
solvent volume (Procedure B), cooperative testing was done on X1.2 The ranges
ranges used for the precisio
precision
n were as follows:
follows:
samples covering a wide range of types of oils, of additive X1.2.1   Fresh Oils— Base numbers from 6 to 70.
concen
con centra
trates
tes whi
which
ch are use
used
d to pre
prepar
paree the
these
se oil
oils,
s, and of  X1.2.2   Additive Concentratess—B
Concentrate —Bas
asee nu
numb
mber
erss fr
from
om 5 to
services for the oils. Even so, however, it was not possible to 300.
cover the complete range of base numbers. It is believed that X1.2.3   Used Oils on Which Were Employed the Forward 
reasonabl
reasonablee inter
interpolat
polation
ion and extr
extrapola
apolation
tion from the rang ranges
es Titration—Base numbers from 5 to 27.

X2. AL
ALTERNATIVE
TERNATIVE SOLVENT
SOLVENT

X2.1 In order to elimina

eliminate
te the chloroben
chlorobenzene
zene from
from this test values
valu es co
cove
vere
red
d a ra
rang
ngee fr
from
om ap
appr
prox
oxim
imatatel
ely
y 0.
0.5
5 to 40400.
0.
method, an alte
method, alternat
rnative
ive solve
solvent
nt was deve
developed
loped.. Coope
Cooperati
rative
ve Statistical analysis of round robin results are available in the
testing was done on samples covering a wide range of types of  research report.6
oils, both new and used, and of additive concentrates used to X2.5.2   Repeatability—The difference between two test re-
prepare these oils. Results have shown that the two solvents sults, obtained by the same operator with the same apparatus
provide statistically equivalent results; however, the precision under constant operating conditions on identical test material,
of the alternative solvent is worse than the original. Paragraph would, in the long run, in the normal and correct operation of 
X2.5
X2 .5.5
.5 de
desc
scri
ribe
bess ho
how
w to co comp
mpar
aree re
resu
sult
ltss us
usin
ing
g th
thee tw
twoo the test method, exceed the following values only in one case
different
different solvents. in twenty:
6.2 % of the mean
X2.2 Rege
Regents
nts
X2.2.1   Xylenes, mix ixeed. (Warning
Warning—Flammable.
—Flammable. Vapor NOTE   X2.1—A
X2.1—Ass par
partt of the same rou
round
nd rob
robin,
in, these sam
samples
ples were
analyzed using chlorobenzene. The repeatability using chlorobenzene was
harmful.) calculated to be 3.4 % of the mean.
X2.2.2   Altern
Alternative
ative Tit
Titration
ration Solvent —Add one volume of 
Solvent 
X2.5.3   Reproducibility—The difference between two single
glacial acetic acid to two volumes of mixed xylenes.
and independent results obtained by different operators work-
X2.3 Proc
Procedur
eduree ing in different laboratories on identical test material would, in
the long run, in the normal and correct operation of the test
X2.3.1
X2. 3.1 Pro
Proced
cedure
ure A of Test Met
Method
hod D 289
2896 6 is fol
follow
lowed
ed
method
met hod,, exc
exceed
eed the fol
follow
lowing
ing values
values onl
onlyy in one case in
exactly, except that mixed xylenes replace chlorobenzene and
twenty:
the alternative titration solvent replaces the titration solvent.
16.2 % of the mean
X2.4 Repor
Reportt NOTE  X2.2—As part of the same round robin, the same samples were
X2.4.1 Repor
Reportt the result as follows: analyzed using chlorobenzene. The reproducibility using chlorobenzene
was calculated to be 8.7 % of the mean.
Base Number  ~ Test Method D 2896–Alternative Solvent, X2 ! 5  Result
X2.5.4   Relative
Relative Bias—No sys
system
temati
aticc bia
biass was det
detect
ected
ed
X2.5 Prec
Precisio
ision
n and Bias between the chlorobenzene and mixed xylenes methods.
X2.5.1 The precision and bias of this alternative
alternative solvent test
method was determined through a round robin using new and 6
Supporting
Supporting data have been filed at ASTM International
International Headquarters and may
used oils as well as additive concentrates. The base number be obtained by requesting Research Report RR: D02-1345.

7
 

D 2896 – 03
X2.5.5 To compare
compare results obtained using different
different solvents, 5.0 % of the mean
use the following: X2.5.5.2   Reproducibility—Th
—Thee dif
differ
ferenc
encee bet
betwee
ween
n two
X2.5.5.1   Repeatability—Th
—Thee dif
differ
ferenc
encee bet
betwee
ween n two tes
testt single and independent results using the two different solvent
results using the two different solvent systems, obtained by the systems, obtained by different operators working in different
same operator with the same apparatus under constant operat- laboratories on identical test material, would, in the long run, in
ing conditions on identical test material, would, in the long run, the normal and correct operation of the test method, exceed the
in the normal and correct operation of the test method, exceed following values only in one case in twenty:
the following values only in one case in twenty: 13.0 % of the mean

SUMMARY OF CHANGES

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D 2896–01 1) that may impact the use of this standard.
e

(1)   Added type of samples that may be analyzed by this test

method in Note 9.

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