Designation: D 2613 01

Standard Test Method for Calcium or Zinc in Paint Driers by

1
EDTA Method
ThisstandardisissuedunderthexeddesignationD2613;thenumberimmediatelyfollowingthedesignationindicatestheyearof
originaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.A
superscriptepsilon(e)indicatesaneditorialchangesincethelastrevisionorreapproval.

5. Apparatus
1. Scope
5.1 Centrifuge, capable
of developing 1000
1.1 This test method covers a titrimetric
to2000g.
determination of calcium in liquid calcium
driersandzincinliquidzincdriersthatcanbe
dissolved in a toluenealcohol mixture and
utilizes the disodium salt of 1 Thistestmethodisunderthe
ethylenediaminetetraacetic acid dihydrate jurisdiction of ASTM Committee
D01onPaintandRelatedCoatings,
(EDTA).
Materials,andApplicationsandis
1.2 Thistestmethodisnotapplicabletodrier the direct responsibility of
SubcommitteeD01.21onChemical
blends.
Analysis of Paints and Paint
1.3 All cations that can be titrated with Materials.
EDTAinalkalinemediainterfereandmustnot Current edition approved Jan.
10, 2001. Published March 2001.
bepresentinthesample.
Originally published as D 2613
1.4 This standard does not purport to 67T.LastpreviouseditionD2613
e1
2
address all of the safety concerns, if any, 85(1994)
Annual
. Book of ASTM
Standards,Vol06.04.
associatedwithitsuse.Itistheresponsibilityof 3
Annual
Book of ASTM
Standards,Vol11.01.
the user of this standard to establish appro
priate safety and health practices and
Annual Book of ASTM
determine the applicability of regulatory 4Standards,Vol15.05.
limitationspriortouse.

2. ReferencedDocuments
2.1 ASTMStandards:

D600Specicationfor
LiquidPaintDriers2D1193
SpecicationforReagent
Water3

E180PracticeforDeterminingthePrecisionof
ASTMMethodsforAnalysisandTestingof
IndustrialChemicals4

E300PracticeforSamplingIndustrial
Chemicals4

3. SummaryofTestMethod
3.1 The liquid calcium or zinc drier is
dissolved in toluene and ethyl alcohol and
treated with an excess of standard EDTA
solution.Theexcessistitratedwithastandard
zincchloridesolutionusingEriochromeBlack
Tastheindicator.

4. SignicanceandUse
4.1 Thistestmethodmaybeusedtoconrm

thestatedcalciumorzinccontentofpureliquid
calcium or zinc driers soluble in toluene
alcohol and manufactured for use by the
coatingsindustry.

6. Reagents
6.1 Purity

of
ReagentsReagent grade
chemicalsshallbeusedin
alltests.Unlessotherwise
indicated, it is intended
that all reagents shall
conform to the
specications of the
Committee on Analytical
ReagentsoftheAmerican
Chemical Society, where
such specications are
available.5 Other grades
maybeused,provideditis
rst ascertained that the
reagent is of sufficiently
high purity to permit its
use without lessening the
accuracy of the
determination.
6.2 Purity

of
WaterUnless otherwise
indicated, references to
water shall beunderstood
to mean reagent water
conforming to Type II of
SpecicationD1193.
6.3 Buffer
SolutionAdd 350mLof
concentrated ammonium
hydroxide(NH4OH,spgr
0.90) to 54 g of
ammonium chloride
(NH4Cl)anddiluteto1L
withwater.
6.4 EDTA, Standard
Solution(0.05M)Weigh
18.62gofEDTA,dissolve
inwateranddiluteto1L.
Storeinapolyethyleneor
borosilicateglassbottle.
6.5 Indicator
MixtureTriturate0.2gof
Eriochrome BlackT and
100gofsodium chloride
(NaCl) and store the
mixture in a tightly
stoppered bottle. This
mixtureremainsstablefor
severalyears.

6.6 Zinc Chloride, Standard Solution (0.05 NOTE 1Liquid driers are
M)Weigh 3.2690gofzincmetal to0.5mg normallyhomogeneoussothat
and dissolve in 50 mL of dilute hydrochloric onlysimplephysicaltests,such
acid(14mLofconcentratedHCl(spgr1.42)to as specic gravity or solids
36mLofwater).Warmifnecessary.Diluteto1 content, on top and bottom
samples from tanks, are
Linavolumetricask.
required to conrm that

separation has not occurred.

7. Sampling
Agitate drums in accordance
7.1 Takeasmallsampleofliquiddrierfrom with the section on Tube

bulk using the procedures in Practice E 300SamplingofPracticeE300.

appropriateforthesizeofthecontainer:Section 7.2Examinethesample
19 for tanks and tank cars or Section 23 for ofdrierforsedimentor
drumsandcans.
1

suspended
5
ReagentChemicals,American
Chemical Society Specications,
American Chemical Society,
Washington, DC. For suggestions
onthetestingofreagentsnotlisted
bytheAmericanChemicalSociety,
see Analar Standards for
Laboratory Chemicals, BDH Ltd.,
Poole,Dorset,U.K.,andtheUnited
StatesPharmacopeiaandNational
Formulary, U.S. Pharmacopeial
Convention, Inc. (USPC),
Rockville,MD.

Copyright ASTM, 100 Barr

Harbor Drive, West

Conshohocken, PA 19428-2959,
United States.

D
matterwhichifpresentisevidenceofnoncompliancewith
SpecicationD600.

EDTAsolutionintoeachbeaker.Add15mLofbuffersolution
and0.20goftheindicatormixture(moreorlesscanbeadded,
if desired). Mix thoroughly by swirling. Titrate with the
standard ZnCl2 solutionto the rst permanent tinge of red.
Maintain vigorous swirling during the titration to ensure
thoroughmixingofthetwophaseswhichmayappear.

7.3Ifthesampleishomogeneouskeepitinastoppered
vesseltopreventsolventevaporationpriortoanalysis.
8.Standardization

2613

8.1ZincChlorideStandardSolution(0.05M)Calculate
theexactmolarity,M1,ofthesolutionasfollows:
M15S1/65.37

(1)

where:

= zincused,g,and
65.37 = zinctoproducea1Msolution,g/L.
8.2
EDTA,StandardSolution(0.05M)Measure40.0mL
oftheEDTAsolutionintoa250mLaskthatcontains10mL
oftolueneand100mLof95%ethylalcoholpureordenatured.
Add15mLofbuffersolution,0.2gofindicatormixture,and
mixthoroughly.Titratewiththestandardzincsolutiontothe
rstpermanentappearanceofaredcolor.
9.Procedure
8.2.1CalculatethemolarityoftheEDTAsolution,M2,as
follows:
S1

M25~V13M1!/40.0

where:

V1

40.0

(2)

= ZnCl2solution,mL,
=EDTAsolutiontitrated,mL.

9.1
Checktheclarityofthedrier.Ifnotclear,centrifugea
portionofthesampleuntilitisclear.Keepthecentrifugetube
stopperedsothatthesolventwillnotevaporate.
9.2
Fromaburetplaceafewgramsofthedrierina50mL
Erlenmeyeraskthatisttedwithacorkthroughwhichpasses
adroppingtubeandrubberbulboreyedropperandobtainthe
totalweight.Weighbydifferencetwoorthree1gspecimens
(10dropsweighabout0.2g)tothenearest0.5mginto400mL
assaybeakersorwidemouthasks(Note2).Add10mLof
toluenetoeachspecimenandswirltomix.Add100mLof
95%ethylalcoholandswirlagainuntilthespecimenis
dissolvedandwelldispersed.Fromaburetmeasure40.0mLof

NOTE 2Ifamagneticstirrerisavailable,itisconvenienttotitratein
anordinarybeaker.Stirringmagneticallyensuresthoroughmixingduring
thetitration.
NOTE3Iftheendpointisoverstepped,add1.0mLoftheEDTA
solutiontothemixtureandtitrateagainwithstandardZnCl 2solution.Use
totalvolumeofeachsolutionforthecalculation.

10.Calculation
10.1 CalculatethepercentofCa,A,orZn,B,asfollows:

where:
V2
=
V3
=
S
=
4.01 =
6.54 =

A5@@~V2M2!2~V3M1!#4.01#/S

(3)

B5@@~V2M2!2~V3M1!#6.54#/S

(4)

EDTAsolution,mL,

ZnCl2solutionrequiredforspecimen,mL,

specimenused,g,
millimolarweightofCa3100,and
millimolarweightofZn3100.

11.PrecisionandBias(seePracticeE180)
11.1 Precision:
11.1.1 RepeatabilityTworesults,eachthemeanofdupli
catedeterminations,obtainedbythesameoperatorondifferent
daysshouldbeconsideredsuspectiftheydifferbymorethan
0.05%calciumorzinc.
11.1.2 ReproducibilityTworesults,eachthemeanofdu
plicatedeterminations,obtainedbyoperatorsindifferentlabo
ratoriesshouldbeconsideredsuspectiftheydifferbymore
than0.10%calciumorzinc.
11.2 BiasBiascannotbedeterminedbecausethereareno
acceptedstandardsforcalciumandzincinpaintdriers.
12.Keywords
12.1 calcium;drieranalysis;EDTAanalysis;zinc

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