Designation: D 974-08
TP. _ Designation: 139/98
Standard Test Method for
Acid and Base Number by Color-Indicator Titration’
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1. Seopet
1.1 This test method covers the determination of acidic or
basic constituents (Note 1) in petroleum products? and lube
teats soluble or nearly soluble in mixtures of toluene and
isopropyl alcohol. I is applicable fr the determination of acids
‘or bases whose dissociation constants in water are larger than
10°"; extremely weak acids or bases whose dissociation
‘constants are smaller than 10"? do not interfere. Salis react if
their hydrolysis constants are larger than 10°”
[Nore 1—In new and used oils he consents conridered 10 have
sid charceritice ich ngic and inorganic acs esr, phobic
‘Sompound, lactones, resin al of heavy mera, and 0508 gente
ach nbior: and detergent Simin, coasts eosideed >
have basieproperiesinhad organic and iorzanic bases. amino com
‘pounds, sate of weak ache (ape, bi als of polyalde bases. sas
‘Ot heany metal, and adiion agents Suc as inbliors ané deren
Nove 2-This test method i not sable for mensun
conativents of many basic sivesype hub
D473) canbe used fortis purpose,
1.2 This est method ean be used wo indicate relative changes
shat occur in an oil ducing use under oxidizing conditions.
Although the svrtion is made under definite equilibrium
‘conditions, the method does not measure an absolute acidic or
basie property that can be used to predict performance of an oi
under service conditions. No. general relationship between
‘bearing corrosion and acid or base numbers is known
Nore 3—Oil, such as many eating ot soon ls and siar
compounded ois, oF excessively dasecoored ols that cannot be 23+
Tyzed for acid number by this test muod due to obsewity of the
‘lorndistor end point ca be analyd by Test Method D 64. The acid
Ti et eth we he jacion of ASTM Commie D2 09
ie can ta i pny Sibecme
‘Dan0s on Ans Laas
ine Ih wat eco yale be pit ofthe Sein
‘Commie This tot mat! wan alped aio ASTRGIP sl a 18.
“Cureton ape Joy 20K Panton Aus 2008. Oral
speed 918 Lint pevions en proved 207 ve DST07
‘Shae dy tet tia. lene 2a 5 ight es
split cls igi lola wil Be Toad ui 117
ne
unbers obuined by this colorindicator test method nee not be
‘numerically the wane a those obtained by Test Mth fn, the Base
fumbers obisined by she color india test method weed ot be
‘umescally the sre 4 hove oblate by Test Method D 73 but they
fare geverly of he save oer of magaiuds.
1.3 The values stated in ST units are to be regarded as
standard, No other units of measurement are ineluded in this
standard
14 This standard does not purport 0 address all of te
safety concerns, if any, associated with its use. It is the
responsibilty of the user of tis standard to establish appro:
priate safety and health practices and determine the applica
bility of regulary limitations prior to use
2, Referenced Documents
2.1 ASTI Standards:
1D 117 Guide for Sampling, Test Methods, and Speciiea-
‘Mons tor Electrical insulating Cals oF Fesfoeum Origin
1D 64 “Test Method for Acid Number of Petroleum Products
bby Potentiometric Titration
{193 Specification for Reagent Water
D.A175 Terminology Relating to Petroleum, Petrolewn
Products, and Lubricants
D479 Test Method for Base Number Determination by
Porentiometric Hydrachlorie Acid Titration
3. Terminology
3. Definitions:
3.1.4 acid number, a—ihe quantity of base, expressed in
rlligrams of povassium hydroxide per gram of sample that is
required to titrate a sample to a specified ead point,
3.111 Diseussion—In this test method, the indicator is
_p-napliholbenzein trated 1 a green/green-brown end point in
4 woluene-water-isopropanol solvent.
“Far fos ASTM sa vis the AST wb wun.
oma AST Cre Sere a een Fa ta 9 STL
‘Sends ow tri, tr a= Bom Saray pg
“A Summary of Change setion appenes a the end of this sana,ily v 974-08
3.12 base number, n—the quantity of acid, expressed in
milligeams of potassium hydroxide per gram of sample tat is
fequited to trate @ stinple 10 a specified end point.
Siz Discwssiop-cin this est method, the indietor is
pnaphiholbenzein titted Yo an orange end point i a toluene
‘water isopropanol solvent.
“13 used oil, any oll that has bean in a piece of
ceguipment (Cor example, an engine, gearbox, transformes, oF
furbine) whether operated or not. baits
3.2 Definitions of Terms Specific to This Standard:
321 strong eid number, a—he quantity of base, ex
pressed in milligrams of potassium hydroxide per gram of
ample, that is required to Gute a hot water extract of the
Sample {0 ® golden-brovn end point using methyl orange
solution
4, Summary of Test Method
44.1 To determine the acid or base number, the sample is
Gissolved ina mixture of roluene and isopropyl alcohol
‘containing a small amount of wate, and the resulting single-
pase solution is tiated at room temperature with standard
Flcohotic base or alecholie acid solution, respectively, the
fend point indicated by the color change of the added
jp naphaholbenzein solution (orange in acid and green-brovn in
base). To determine the stfong acid number, a separate portion
fof the sample is extracted with hot water and the aqueous
fxtract is rated with potassium hydroxide solution, using
methyl orange as an indicator
5. Signifieance and Use
5.1 Slow and oped potenti products ean contain basie oF
acidic constituents that are present as additives or as dearada
tion products formed during service, such as oxidation prod
tos. The relative amount of these materials ean be devermined
by titrating with acids or bases. This numbes, whether ex:
pressed as acid number oF base number, is a measure of this
mount of acidic or basic substances, respectively, in the
Dilalways under thé conditions of the test, This mamber is
fused as a guide inthe quality control of lubricating oil
formulations. It is also sometimes used as a measure of
Tubrieant degradetio® in service; however, any condemning
Jimits must be enipifeally establishes.
32 Since a variefy of Saidation products contribute t0 the
acid numer and the orgs acids vary widely in corrosive
properties, the test cannot bé used 10 predict cosrosiveness of
fin oil ander sérvice conditions. No general correlation is
Knowa betweenracid number and the corosive tendency of oils
Toward metals. Compounded engine oils can and usvally do
have both acid and base numbers in this test method.
6 Apparatus
6.1 Bure (with the following dimensions
‘smb gaeute ink tens
‘Dink ure asiened 90S or sma wiser
Swi Oz sbowsors
Nose 4—An automate burt capable of devring sant amounts
‘odsmit oe smaller nsenonts ct be used bu he stated precision deta
‘were abisned sing manual butts oy.
7, Reagents
71 Purity of Reagents—-Reaget grade chemicals shall 6&
sed inal tess, Unless otherwise indicated, iis ntended that
lll weagents shail conform to the specifications ofthe Commit
tee on Analytical Reagents of the American Chemical Society
‘Shere such specifications are available* Other grades may be
ised, provided it is rst ascertained chat the reagent of
afficienity high pority to permit its use without lessening the
accuracy of the determination
F2 Parity af Water-—ReFerenees to water shall be under.
stood yo mean reagent water that meets the requirements of
cither Type I Il, oF Ill of Specification D 1193
"73 Iropropy Alcolol, anhydrous (less than 0.9 % wate)
(Warning—Flammable)
7.4 Hydrochloric Acid Solution, Standard Alcoholic —(0.1
M}_-Mix 9 mi of concentrated hydrochloric acid (Warning
Corrosive, fumes cause ieitation) (HCl, sp gr 819) with 1000
fn of anbydrous isopropy! alcobol (2-propanol) (Warning —
Boe 7.3). Standardize frequently enough to detect molarity
changes of 0.0005 (Note 6), preferably by electromesric
titration of approximately 8 ml- (accurately measured) of the
{0.1 M leoholic KOH solution diluted with 125 ml. of carbon
tioxie-free water. When an electrometric titration is used (or
the standardization, the ead point shall be a well-defined
Jnifeetion point closest to the cell voltage for the acidic buffer
Solution, When a colorimetric ization is used forthe standaré-
jnanion, irate to the first stable appearance of the orange color
with aethyl orange indicator
Non: 5—Coninercaly avaiable reagents nay be wed in pce of he
ameatoy pepratian eon thy ne et be corde
one 6 sili cleans, bo the standard KOH and HCH
sofa can bs ssed 0 tht 100 tL is eau to 3.0) mg ot
ROH Sodan bydeoside (MMOH) and sulfur acid (H,SO,) can Be
[nats for KOH and BCL especively
75 Methyl Orange Indicator Soturion—Dissolve 0.1 8 of
ethyl orange in 100 mL of water
7.6 p-Nuphiholvenzein Indivator®* Solution The
_pnapbtholbenzin shall meet the specifications given in Annex
(AI: Prepave solution of p-naphubelbencein in tiation solvent
equal 1 10 £001 pi.
77. Potassium Hydroxide Solution, Standard Alcoholic (0.1
M)_Add 6 gof solid KOH (Warning —Highly corrosive to all
tbody tissue) to approximately 1 L of anhydrous
alcohol (containing Tess than 0.9 water) in a 2-L Erle
flask Boil the misture gently for 10 to 15 min, stirring to
prevent the solids from forming a cake on the botiom, Ad@ at
Menst 2g. of barium hydroxide (BaOH)) (Warning—
Tepe Cheats Americ Chea Sis Spc Ames
con Sven Masten BC, For Sezai om ees oem
Gee Renan Choice Sosy occa Sudo (sna
Trea tats Be: Danes UX ame te Che Se Pree
cet Pande US. Pamaopeid Coan. USPC, Rach
mo,
22006 say. ony Kak ker (Malnhe Faka and Ach wee
om na cons Asa X- Howes Kod ba mo es
ole,
tering he nS AST nnd ean: ly 0974-03
Poisonous if ngesé strongly alkaline, causes severe }itaion
ducing dermatitis} and-agan boil gently for 5 to 10 min
‘Cool to room temperature, allow to stand for several hours, and.
Alter the supenaiant Tiga through a fine sintered-tass oF
porcelain Gerig Tnnel, avoid. unnecessary exposure 10
axibondioride (CO) during filtration Store the solution in a
chemically esistan dispensing bottle out of contact with cork
rubber, of saponifiable topeack lubricant and protected by &
ard tube containing soda lime or soda nontbvous silicate
absorbent (Ascarite, Crbosorb, or Indecsb)
741 Standardization of Potassium Hydroxide Sotution—
Siandaedize frequently enough to detect changes of 0.0005 N.
(One way todo this i as follows: Weigh, tothe nearest 0.1 mg,
approximately 0.2 g of potassium acid phihalate, which has
been dried for atleast 1h at 110 + 14C and dissolve in 40
Tomb of water, free of COs, Titre with the potassium
hydroxide alcoholic solution to either of the following end
points: (2) When the titration is electromettic, tate to a
well-defined infletion point atthe voltage that corresponds 19 |
the voltage ofthe basi buffer solution, or (2) When titration is
add six drops of phenolphinalein indicator solu-
Xe t0 the appearance of @ permanent pink colo.
Perform the blank titration on the water used to dissolve the
powssium acid phthalate, Caleulae the normality using the
fotowing equation:
Wy 1000)
Nomatiy = spn Pe o
weight of the potassium acid phthalate, g,
‘molecular weight ofthe potassium acid phthalate,
‘volume of titrant used 0 tate the salt to the
specie end porat, mL, ana
V, = volume of titrant used to titrate the blank, re
4.1.2 Prepare 10.1 = 0.01 mt solution of phenolphthalein
by dissolving pure solid phenolphihatein in a 1:1 mixture of
‘water, fee of CO, aud ethanol.
ors 1—Cormerily rie agen my eed inp te
tery pean
Nove Bete th aly ge coe fai expan
af eget eo propyl he sand ache
‘Santer sh sence pases cease
inte aon of staple
18 Tiron Solient—Piepare by mixing tluene, wir,
3 anyérts oprpyt alec nthe ro 100: 199
8. Preparation af Used Oil Samples
8.1 Stit observance ofthe sampling procedure deserved
in 62 is necesny since the sediment isl is acti or baie
or has adsorbed soiie of bise material from the sample.
Failure to obsin a representative sample cases serio evors.
8.2 Heat the simple oie 9) of use oil 1060 = 8°C in the
original container and agitate until all sediment if homoge-
‘ously suspended inthe ol (Nore 10) I the ogi Sonainer
is of opaque mate ors i more than three-fourths fll
transfer the envite sample fo a clear glss hoe having
apacty et east one third. grater than the volume of the
sample, snd testy all trices of seciment from the original
container othe bate by violent ataton of potions of the
TABLE 1 Size of Sample!
Tad Naor Brea “easinay a
ase Numer sampn.g __Wesheg 2
Tera
Wea 20220 oa
Oea50 10280 20202 Ed
Ser 25016 2500 53 = 002 Boor
Tae Oa Tes Oe
Wwe 20°02 Tar
‘Over 2516 2500 02 = 002 en:
7 gh canes samples ow asd manta pam wa ol asamp o
‘utsnmore pisces aus The eavpn sooo cnc alse bra othe
‘uinty speotod minnie posse rerence bye ert clr
sample in the original container. After complete suspension of
all sediment, strain the sample oF a convenient aliqust through
44 100-mesh’ screen for the removal of large contaminating
Panicles (Note 9),
None 9--Wken samples are visibly free of sediment, the eating
procedutedescrted it 2 may be omied. When samples ae visibly
Df sient, the esining predce may ao be emt
Dore 10—As used oil can change oppreibly in ste, samples
shold be test ss s00n a8 posible flr removal rom the lubctng
system andthe dates of sampling an esting should Be nt,
9. Procedure for Acid Nomber
5.1 Ino an appropriate size Erlenmeyer Mask or a beaks
introduce a weighed quantity of the sarple as given ia Table
‘Add 100 mL-of the titration solvent and 0.5 ml-o the indicator
solution, and without stoppering, swirl until the sample is
tentiely dissolved by the solvent, If the mixture assures a
yellow-orange color, proceed as directed in 9.2 iF it becomes
Teen or green-black, proceed as directed in Section 10,
Nim, 11—In oun aay th actor may Be pre-med with dhe
tivation solve before adn to he sane
9.2. Without delay, irate ata temperature below 30°C (Sie
14), Add 0.1 M KOH solution in increments and mix 10
disperse the KOH as necessary (ee Note 12). Shake vigor-
‘ously near the end point, but avoid dissolving carbon dioxide
(CO) in the solvent, (In the case of acidic ols, the orange
‘color changes 10 8 green or green-brown as the end point is
approached.) When the solution first urns green or green
‘brown, reduce the increment size to dropwise (manual buret) or
‘pesween 0.01 and 0.05 mL (automated buret). Continue until
persistent green or green-brown end point is reached (see Nove
13) an held fora minimur of 13 s alter the addition of the lst
‘Inorement or if It reverses with two drops of 0.1 Mf HCL
[Non 12--Whon ae numbers abot oslo one re expected eter
cin ca be obined by sbstuting 0.01 gr 008 solations in) >
fd 9.8. This substation wns ot sacladed in he development of
precision xaement
[Nore 13-To aber the epi of darko i, take the Hak
igoroaly vo prodace momontcly a sight foam when Ie clr hangs
‘veut the asf drops of an are added ad serve the tao
hoeescon amp at bec top lve
Nott 14--The epee ca be inured By any wetable taper
we measuring device
Nore 1S-An suiomated photomtrie device may ao be sed ode
the iain end pil However, te precision estimates given in Seton
1S ay no ply thie roc of rationGy o 974-08
93 Blank—Perform a blank tration on 100 mL, of the
sitation solvent and 0.5 mL of the indicator solution, adding
Dil-ml of less increments of the 0.1 M KOH solution
95.1 The titration solvent usually contains weak acid iat
portcs which react withthe strongly basic components of the
ample. To correet the base number forthe sample, determine
fan acid number blank upon the solvent
10, Procedure for Base Number
10.1 If the titration solvent containing the dissolved sample
assumes a green or greenish-bvown color after he indicator is
‘added (0.1), earry ou the titration as described in 9.2, bu use
(.1 AF HICI and Grate until the green-brovn color changes (0
orang.
10.2. Blank—Perform a blank titration as directed in 9.3,
11, Procedure for Strong Acid Number
11.1 Introduce approximately 25 g of a represcatative
sample, weighed tothe nearest 0.1 gy ilo a 250-mL separatory
funnel and add 100 mL of boiling water, Shake vigorousty and
Grain the water phase, alier separation, into a 300-mL. casse~
tole. Exvact the sample twice more with 50-ml. portions of
boiling water, adding both extracts to the casserole, To the
combined extracts add 0.1 mL of methyl orange indicator
Sclution and, if the solution becomes pink or red, titrate with
{0.1 4 KOM solution uni the solution becomes golden brown
in color ff the intial colori not pink or fe report the scons
eid number as zero. (See Note 15.)
12 Blank--Inio a 250-ml. Erlenmeyer flask, introduce 200,
iL of the same boiling water as used forthe sample titration.
‘Add O.1 mL of methyl orange indicator solution. 1 vhe
aca color Is yethyw-urange, styte wih 01 M HET 0 the
“ame depth and shape of color obtained in the titration of the
Sample, If he indicator color is pink or red, state with 0.1 M
KOH solution co the same end point xs that wsed in the sample
tiation.
12, Quality Control, Cheeks
12.1 Confiem the= performance of the equipment oF the
procedure each day it in use, by analyzing a quality control
FOC) sample. Itis advisable to analyze additional QC samples
fs approprint, such as atthe end of abateh of samples oF after
4 fixed number of samples o ensure the quality of the resus
“Analysis of results from these QC samples can be carried Out
ising eoriol chart techniques.” Wiien the result of a teS ot! @
{OC sample exceeds the control limits of the laboratory.
Cconective action, such as, instrament recalibration maybe
Tequived. An ample'svpply of QC sampte material shall be
tvailable forthe intended period of use, and shall be homoge-
neous and stable under the anticipated storage conditions. 1f
possible, the QC sample sball be representative of samples
Aypieally analyzed and the average value and conto limits of
the QC sample shall be determined prior to monitoring the
measurements process, The precision for the QC sample must
TN 3 tal en eso of Das Col Cho Aus Seo
cone se mes ih, ASTM eran, W. Coase.
bbe compared agsinst that given in the Precision and Bins
ection ofthis test method in oréer to verify that de insrument
is functioning correctly
Nowe 16--Bocose the acid and base numbers ean vey while the QC
samples storage, when an opof-orto suaon ares he abit
‘re QC snl cam be a SOE ofthe eos
13, Calteulation
13.1 Coleutate the aeid number as follows
‘aed aber. my of KOM = (A = BMX SOTA
where:
JE KOH solution required for tration of the sample
(92), mL,
1B = ROH solution required for tration of the blank (9.2).
ml,
AM = molarity of the KOH solution, ang
W = sample used, 2
13.2 Caleulate the seong-acid number as follows:
13.21 Ifthe blank ttvaion is made with acid
‘strong uber, ng of KORVg = (CM + Dr) % S61
8
where:
CS KOH solution required to titrate the water extract
tH. be ml,
M--= molarity of KOH solution,
= HCL solution required (0 titra the blank solution
(112), ob,
im = molarity of the HCI solution, and
W> = sample used, g
15.2.2 If the blank titation is made with base:
‘trong acid manor. ng. of KOWg = [C~ BEX 30H
where :
CE KOH solution required 10 titre the water extack
Cem,
= KOH solution required 10 strate the blank solution
(1D. oe,
M_ = inolarity of the KOH solution, and
W> = sample used,
133 Calculate the base number as follows
tise suber. mg of KOH = (Em + FB x S61VW (8)
where
Ee HCI solution required for titation of the sample
(Seetion 10). mb,
iv molary of the FICL sofotion
P= KOH required for ation of the acid number blank,
mi;
M_ = moiarity of the KOH solution. and
W = sample used, g
14, Report
TMiL Report the resell as acid number strong acid number
‘or base number as Follows:
‘a ms (DTA = we
sang ar (D9) =)
eve mer (D9 EG)lp 0074-08
15, Precision and Bias
15.1 Precisian—This precision section applies only to new,
light-colored, straight mineral oils and new and used inhibited
stenm turbine oils. Insulicient data are available on other oils
coming within the scope ofthis ist method so that no precision
is given for such els.
15.1.1 Repeabiliry—The difference between two test re-
sults, obtained by the same operator with the same. apparatus
‘under constant operating gpnditions on identical test material,
would in the long wun, in the normal and correct operation of
te test method, exceed the following values only in one case
in weniy:
ox Bate Niner eget
‘oooion ‘O08
Ore 84 05 203
be 05 8 to oe
Ove 1 20 be
15.1.2 Reproducibiliy—The difference between two single
and independent results obtained by diffevent operators worke
ing indifferent laboratories on identical test material would, in
‘the long run, in the narmal and correct operation of the test
method, exceed the following values only in one case in
twenty:
Dos 0 Nomar oprecucity
‘oaowan ae
Orer 8008 oo
Barese20 15% oliheneuetaton
None 17—Tneve reison wakes dona ppl is ha a hia
colored aso obuate the en pint eee change
[Nowe 18-—For peeision applicable 1 lec insaating qu, refer
ve Guide D117
‘None 19-The pression statements were based on the we of manual
twrets ony The wri eataned sha the precision samen my oF |
‘may no be eplizable to tations perfeaned with te use of atte |
{rcs ince inetiborory study fas been condiced to dle 10
‘tiislly evaleate tule determined by both ecnigues.
15.2 Blas—The procedures inthis west method have no bias
because the acid and base values can be defined only in the
terms of the test method.
16, Keywords
16.1 acid number; base number; color indication titration;
petroleum products
ANNEXES
«Mandatory Information)
BH Al, SPECIFICATIONS FOR p-NAPHTHOLBENZEIN
AL1 pNaphuholhenzein shall conform to the following
requirements
Alslel Appecrance—Red amorphous powder.
ALLL2 Chlarides-—Less than 0.5%.
AL.1.3 Solubiliqy—Ten grams shall dissolve completely in|
of tiation solvent (see 42.7.3)
AL.L.4 Miniowm Absorbance—Bxactly 0.1000 g of sample
is dissolved in 250 mL. of methanol. (Warning—Flammable.
‘Vapor harmful, Can be fatal or cause Blindness if swallowed or
inaled. Cannot be made nonpoisonous.) Five mililtes ofthis
solution i8 made wp to 100 mL with pH 12 buffer. This final
dilution should have a minimum absorbance of 1.20 when read
atthe 650-nm peak using 1 Beckman DU or altemative type
speettophiotometer, I-em cells, and water as the blank.
‘ALLS pH Range:
2, TEST METHOD FOR DETERMINING ple RANGE OF p-NAPHTHOLBENZ
ALL Seope
AQI.I This test method is intended for deiermining the
acceptability of p-naphtholberzcin indicator for use in Test
Methad D974 with regard to color change over a per range.
A22. Terminology
A22.1 Definitions of Terms Specific ro This Standard:
AMLI.5.1 Indicator turns tothe fist clear seen ta relative
pH of 11 0.5 when tested by the method for pHr range of
_penaphiholbenvzein indicator as described in Nowe A
AILI.5.2 Requites not more than 03 mL of 001 44 KOH
solution above that for blank to bring indicator solution 10 the
first clear green.
ALL.53 Requires not more than 1.0 mL of 001 M KOH
solution ebove that for blank to bring indicator solution 10 a
blue color.
AL1.S.t Initial pH of indicator solution is atleast as high
8 that of the blank
AL15.5 Buller is made by mixing SO mL of 0.05 HF
iabasie Sodium phosphate solution with 269 mL. of 0.1 Af
sodium hydroxide solution
INDICATOR
AQ2I.A pir, man arbitrary term which expresses the
relative hydrogen fon activity inthe toluene-isopropanol-water
smedinm,
A22.1.1L Discussion—For the purpose ofthis test method,
the pls acidity Seale is defined by two standard buffer solutions
whieh have been designated pHlr 4 and pHr 11, The exact
relation berween pHr and the true pH of a toluene-sopropancl-
‘water solution is not known and cannot be readily determined,dy 0 974-08
A23 Summary of Test Method
[A23.1 A prescribed amount of indicator is trated electro:
metrically through the various color changes with aleaholie
{(Warning—Flaminable) potassium hydroxide and results plot
ted against meter readings converted to pHr units.
A2A Significance and Use
'A24.1 This procedure is used to establih the pHr values of
the various color changes of the p-napinholbenzein indicator,
A2S Apparatus
‘ALS Meter, Glass Blectrode, Calomel Electrode, Strre
Beaker and Stand, as specified inthe Apparat section of Test
Method D 64,
A26 Purity of Reagents
'A26.1 Reagent grade chemicals shall be used in all tests
‘Unless otherwise indicated, itis intended that all reagents shal
tonform to the specifietions of the Commitee on Analytical
Reagents of the American Chemical Society, where, such
spociicaions are avilable’ Other grades may be used pro-
ded itis Gest ascereined shat the reagent is of sufficiently
igh purty to permit its use without lessening the accuracy of
the determination
“22.62 Relerences to water shall be understood to mean
isilled water.
A27 Reagents
‘A227. Potassium Hydroxide Solution, Standard Atcolic
00 at) —Prepre, soe. and sandaize In accordance with
{est Method 6b
Se ftesttorie Ast Sluinn Standort Ache (0.2
Mp Prapar and sangre in aocorance wily Test Method
Dees
523 raion Solven—Add $00 ml-of toluene and 5
ot Water (0 498 mL of anhydrous. opropy! aleohol 2
fropanoly The tion solves should be made up in are
Suances
11 Acide Ber Solution (ptr = 4.0}—Prepte a stock
solntion i asordane with Tet Method D 068, Add 10 eof
‘Rite sock soton to. 100-ml of Giraion solves. Use the
diluted solution within 1.
a7 aleline Bujer Solin (pHr= 1-0)—Prepare &
sjsu aouton in accordance with Test Method D 664. Add 10
Mic of buffer sock slution wo 100 Lofton solvent. Use
the ited slion within 1
“A216 Powann Chloride Elecrolyre—Prepare & sato-
sated sation of potassium eilorde (KCI In wate.
S277 NaphitelberceinPuicaor Soliton Prepare as =
sotied in 7
‘A2.8 Preparation of Electrode System
'A2B.L Prepare the electrode systent in accordance. with
“section 8, Preparation ofthe Blectrode System, of Test Method
B66,
429 Standardization of Apparatus
'A2S9.1 Prior to each tes{ oF series of tests, set the meter 10
read) on the pH seale, insert the electrodes imo beaker
1G, Az Calibration Curve for Conversion of pH Meter Reasngs
to pHr
containing the acidie nonaqueous buffer solution at» tempers:
fue of 25 = 2°C. and stirthe solution vigorously. When the pH
moter reading becomes constant adjust the asymmetty potential
‘ind of the instrument so thatthe meter reads 4.0.
"42.9.2 Remove the acidic buffer, clean the electrodes. and
immerse them in water for several minutes. Dry the elecwodes
find ingest them in a beaker containing alkaline conaquects
buffer solution at 25 = 2°C. When the pl¥ meter reading has
become sadly, record the exact value. Ifthe reading is within
02 pH units of 11.0, the inital acidity, pHe, of unknown
Solutions may be read directly from the dial ofthe meter. IF the
aang i not swith 0.2 units of 11.0, prepare s correction
fpeph as shown in Fig. A2.1. Use this graph to convert pit
Soter sasings tintin acidity. pl
A210 Procedure
‘A21O.1 Tite 100 mL of titration solvent (Warn
Framinable) with 001 M KOH. solution ntl the meter
indicates a pH berween 13 and 14
“AZ 10.2 Add 0.5 mi. of indicator solution toa fresh portion
of tiation solvent, and afer cleaning the electoses titrate with
Lot A KOH solution wnil dhe meter indicates a pHr between
Sand 14.
[ADIOS During the titration, plot the volume of ivan
against the pit oF meter reading and aote on the curve the
various color cianges atthe coresponding pH values
‘Now A21-Fe following coor csnges. in ones ae inlended 8 =
eve
‘ante ave ren
Ove geo chara
‘her geo BE
ha en 1 8
|A2.104 Plot the blank ttsation on the same paper used (oe
te indicator
A2A1 Caleulatio
‘A211 Subtract the volume of titrant used in the blak
sation from that used forthe indicaor solution ttsation at the
amv pil corresponding tothe definite color changes betwee!
10 to 12 pleGly v 974-08
A212 Precision and Bias A2.I2.2 Bias—The proceduces in this test method have no
‘A221 Pregision—The precision ofthis procedure has aot bits because the values can only be defined in terms of the test
been determined, and there are no plans 10 develop one method.
SUMMARY OF CHANGES
Subcommittee 102.06 bas identified the location of selected changes to this standard since the last issue
(0974-07) that may impact the use ofthis standard. (Approved July I, 2008.)
() Expanded 9.2 to clarify the color end poi
‘Subcommittee 102.06 has identified the locaton of selected changeS to this standard since the last issue
(8974-06) thas may impact the use of this standard, (Approved Nov. 1. 2007.)
(7) Added Footaté$ indicating current availabilty of eeagent (2) Added RR:DO2-1626.
‘p-naphiholben2ein indicator,
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