ASTM D2351-90(1999)

Standard Test Method for Sulfide in White Pigment Separated from Solvent-Reducible Paints

SCOPE
1.1 This test method covers the determination of sulfide sulfur in white pigment separated from solvent-reducible paints.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-May-1999
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaced By: ASTM D2351-90(2005) - Standard Test Method for Sulfide in White Pigment Separated from Solvent-Reducible Paints
• Effective Date: 01-Jan-2005

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 2351 – 90 (Reapproved 1999)
Standard Test Method for
Sulfide in White Pigment Separated from Solvent-Reducible
Paints
This standard is issued under the fixed designation D 2351; 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
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
1.1 This test method covers the determination of sulfide
where such specifications are available. Other grades may be
sulfur in white pigment separated from solvent-reducible
used, provided it is first ascertained that the reagent is of
paints.
sufficiently high purity to permit its use without lessening the
1.2 This standard does not purport to address all of the
accuracy of the determination.
safety concerns, if any, associated with its use. It is the
5.2 Purity of Water—Unless otherwise indicated, references
responsibility of the user of this standard to establish appro-
to water shall be understood to mean reagent grade water
priate safety and health practices and determine the applica-
conforming to Type II of Specification D 1193.
bility of regulatory limitations prior to use.
5.3 Ammoniacal Cadmium Chloride or Zinc Sulfate
2. Referenced Documents
Solution—Dissolve8gof cadmium chloride (CdCl ·2H O) in
2 2
200 mL of water and add 200 mL of ammonium hydroxide
2.1 ASTM Standards:
(NH OH, sp gr 0.90); or, dissolve 200 g of zinc sulfate
D 215 Practice for ChemicalAnalysis of White Linseed Oil
(ZnSO ·7H O) in 1080 mL of water and 920 mL of NH OH
2 4
Paints
(sp gr 0.90).
D 1193 Specification for Reagent Water
5.4 Hydrochloric Acid (sp gr 1.19)—Concentrated HCl.
D 2371 Test Method for Pigment Content of Solvent-
5.5 Lead Nitrate, Alkaline Solution— Into 100 mL of
Reducible Paints
potassium hydroxide (KOH) solution (56 g in 140 mL of
3. Summary of Test Method
water)pourasaturatedsolutionofleadnitrate(Pb(NO ) )(250
3 2
g in 500 mLof water) until the precipitate ceases to redissolve,
3.1 The extracted pigment is placed in a flask with mossy
stirring constantly while mixing. Let settle, filter through a
zinc. The hydrogen sulfide generated by addition of HCl reacts
glass filter, and dilute the clear filtrate with an equal volume of
with lead nitrate in an absorption flask forming lead sulfide.
water. About 3 volumes of the Pb(NO ) solution will be
The lead sulfide is dissolved with nitric acid (HNO ) and the
3 2
required for 1 volume of the KOH solution.
lead determined as lead sulfate in accordance with Test
5.6 Mossy Zinc.
Methods D 215.
5.7 Nitric Acid (1+4)—Mix 1 volume of concentrated
3.2 A rapid method is also described.
HNO , (sp gr 1.42) with 4 volumes of water.
4. Significance and Use
5.8 Potassium Iodate, Standard Solution—Dissolve 3.6 g of
potassium iodate (KIO ) and 39 g of potassium iodide (KI) in
4.1 Sulfidecontainingpigmentssuchaslithoponehavebeen
1Lofwater.Forgeneralworkthetheoreticalsulfurtiterofthis
used in paints in varying degrees in the past years. As such it
solution should be used; for special work the solution may be
is useful to formulators and users to be able to monitor the
standardized against similar material, such as a lithopone of
amount of this compound in whole paints.
known sulfide sulfur content. The theoretical titer is based on
5. Reagents
standardsodiumoxalate(Na C O )andisobtainedasfollows:
2 2 4
To 300 mL of water in a 600-mL flask, preferably glass-
5.1 Purity of Reagents—Reagent grade chemicals shall be
stoppered, add 10 mL of HCl (sp gr 1.19) and1gofKI. Cool
used in all tests. Unless otherwise indicated, it is intended that
and add 10 mL of 0.1 N potassium permanganate (KMnO )
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved May 25, 1990. Published July 1990. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 2351 – 65T. Last previous edition D 2351 – 85. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 06.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
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