ASTM D215-91(2002)

Standard Practice for the Chemical Analysis of White Linseed Oil Paints (Withdrawn 2005)

SCOPE
1.1 This practice covers the chemical analysis of the usual white linseed oil paints. The methods included are listed in Table 1.
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.
WITHDRAWN RATIONALE
This practice covers the chemical analysis of the usual white linseed oil paints.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this practice was withdrawn in September 2005. This standard is being withdrawn without replacement due to the fact that this method uses a Gooch crucible lined with asbestos and also that there are no longer manufacturers of white linseed oil paint.

General Information

• Status: Withdrawn
• Publication Date: 14-May-1991
• Withdrawal Date: 20-Sep-2005
• ICS: 87.040 - Paints and varnishes
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaces: ASTM D215-91(1996) - Standard Practice for the Chemical Analysis of White Linseed Oil Paints
• Effective Date: 15-May-1991
• Referred By: ASTM D5146-10(2019) - Standard Guide to Testing Solvent-Borne Architectural Coatings
• Effective Date: 15-May-1991
• Referred By: ASTM D3720-90(2019) - Standard Test Method for Ratio of Anatase to Rutile in Titanium Dioxide Pigments by X-Ray Diffraction
• Effective Date: 15-May-1991
• Referred By: ASTM D6763-16(2022) - Standard Guide for Testing Exterior Wood Stains and Clear Water Repellents
• Effective Date: 15-May-1991
• Referred By: ASTM D49-83(2020) - Standard Test Methods of Chemical Analysis of Red Lead
• Effective Date: 15-May-1991
• Referred By: ASTM D5324-16(2022) - Standard Guide for Testing Water-Borne Architectural Coatings
• Effective Date: 15-May-1991
• Referred By: ASTM D2349-90(2020) - Standard Test Method for Qualitative Determination of Nature of Solvent Composition in Solvent-Reducible Paints
• Effective Date: 15-May-1991
• Referred By: ASTM D1301-91(2020) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 15-May-1991

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:D215–91 (Reapproved 2002)
Standard Practice for the
Chemical Analysis of White Linseed Oil Paints
This standard is issued under the fixed designation D 215; 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.
TABLE 1 List of Test Methods
1. Scope
ASTM
1.1 This practice covers the chemical analysis of the usual
Test Method Section
Method
white linseed oil paints. The methods included are listed in
Preparation of Sample 4 .
Table 1.
Water 5 D 1208
1.2 This standard does not purport to address all of the
Volatile Thinner 6 D 2369
Nature of Thinner 7 D 2349
safety concerns, if any, associated with its use. It is the
Percentage of Pigment 8 D 2371
responsibility of the user of this standard to establish appro-
Percentage of Nonvolatile Vehicle 9 .
priate safety and health practices and determine the applica-
Separation of Vehicle 10 D 2372
Unsaponifiable Matter 11 D 1397
bility of regulatory limitations prior to use.
Fatty Acids 12 D 1398
Iodine Number of Fatty Acids 13 D 1959
2. Referenced Documents
Resin 14 D 1542
Qualitative Analysis, Single, Mixed, or Composite 15 .
2.1 ASTM Standards:
Pigments
D34 Guide for Chemical Analysis of White Pigments
Quantitative Analysis, Single Pigment 16 D34
D50 Test Methods of Chemical Analysis of Yellow, Or-
Quantitative Analysis, Mixed or Composite Pig-
ments:
ange, Red, and Brown Pigments Containing Iron and
Moisture and Other Volatile Matter 17 D 280
Manganese
Loss on Ignition 18 D 1208
D 280 Test Methods for Hygroscopic Moisture (and Other
Insoluble Matter 19 .
Total Lead (Antimony) 20 .
Matter Volatile Under the Test Conditions) in Pigments
Antimony Oxide 21 D 2350
D 717 Test Methods for Analysis of Magnesium Silicate
Soluble Barium 22 .
Pigment Aluminum Oxide 23 .
Total Zinc 24 .
D 1193 Specification for Reagent Water
Soluble Calcium 25 .
D 1208 Test Methods for Common Properties of Certain
Soluble Magnesium 26 .
Pigments
Carbon Dioxide 27 D 1301
Total Soluble Sulfur Compounds 28 D34
D 1301 Test Methods for ChemicalAnalysis of White Lead
Soluble Sulfate 29 D50
Pigments
Sulfide Sulfur 30 D 2351
D 1394 Test Methods for Chemical Analysis of White
Sulfur Dioxide 31 D 2352
Matter Soluble in Water 32 D 1208
Titanium Pigments
D 1397 Test Method for Unsaponifiable Matter in Alkyd
Resins and Resin Solutions
D 2349 Test Method for Qualitative Determination of Na-
D 1398 Test Method for Fatty Acid Content of Alkyd
ture of Solvent Composition in Solvent-Reducible Paints
Resins and Alkyd Resin Solutions
D 2350 Test Method forAntimony Oxide in White Pigment
D 1469 Test Method for Total Rosin Acids Content of
Separated from Solvent-Reducible Paints
Coating Vehicles
D 2351 Test Method for Sulfide in White Pigment Sepa-
D 1542 Test Method for Qualitative Detection of Rosin in
rated from Solvent-Reducible Paints
Varnishes
D 2352 Test Method for Sulfur Dioxide in White Pigment
D 1959 Test Method for Iodine Value of Drying Oils and
Separated from Solvent-Reducible Paints
Fatty Acids
D 2369 Test Method for Volatile Content of Coatings
D 2371 Test Method for Pigment Content of Solvent-
Reducible Paints
This practice is under the jurisdiction of ASTM Committee D01 on Paint and
Related Coatings, Materials, and Applications and is the direct responsibility of
D 2372 Practice for of Separation of Vehicle from Solvent-
Subcommittee D01.21 on Chemical Analysis of Paint and Paint Materials. 4
Reducible Paints
Current edition approved May 15, 1991. Published July 1991. Originally
e1
published as D 215 – 25 T. Last previous edition D 215 – 73 (1979) .
Annual Book of ASTM Standards, Vol 06.03.
3 4
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 06.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D215–91 (2002)
3. Purity of Reagents ANALYSIS OF PAINT
3.1 Reagent grade chemicals shall be used in all tests.
6. Water
Unless otherwise indicated, it is intended that all reagents shall
6.1 Determine water in accordance with Test Methods
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such D 1208.
specifications are available. Other grades may be used, pro-
7. Volatile Thinner
vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
7.1 Determine the volatile matter in accordance with Test
the determination.
Method D 2369. Calculate the loss in weight as the percentage
3.2 Unless otherwise indicated, references to water shall be
of water and volatile thinner. Subtract from this the percentage
understood to mean Type II reagent grade water conforming to
of water as determined in accordance with Section 6. Report
Specification D 1193.
the remainder as percent volatile thinner.
4. Hazards
8. Nature of Thinner
4.1 Ammonium Hydroxide causes severe burns and may be
8.1 Determine the nature of the thinner in accordance with
fatal if swallowed. Read the appropriate Material Safety Data
Test Method D 2349.
Sheets (MSDS) before using.
4.2 HydrochloricandSulfuricAcids causesevereburnsand
9. Percentage of Pigment
may be fatal if swallowed. Read the appropriate MSDS before
9.1 Determinethepercentageofpigmentinaccordancewith
using.
Test Method D 2371. Preserve the pigment as prepared in a
4.3 Acetic Acid causes severe burns and may be fatal if
stoppered bottle for use in Sections 16 and 17.
swallowed. Read the appropriate MSDS before using.
4.4 Nitric Acid causes burns and may be fatal if swallowed.
10. Percentage of Nonvolatile Vehicle
Vapor is extremely hazardous and may cause nitrogen oxide
10.1 Add together the percentages of water, volatile thinner,
poisoning. Read the appropriate MSDS before using.
and pigment, and subtract the sum from 100. Report the
4.5 Toluene is flammable. Vapors are harmful. Use with
remainder as nonvolatile vehicle.
adequateventilation.ReadtheappropriateMSDSbeforeusing.
4.6 Hydrogen Sulfide is both an irritant and an asphyxiant.
TESTING NONVOLATILE VEHICLE
Read the appropriate MSDS before using.
4.7 Ammonium Sulfide evolves hydrogen sulfide on contact
11. Separation of Vehicle
with acid or acid fumes. See 4.6. Read the appropriate MSDS
before using.
11.1 Separate the vehicle from the pigment in accordance
4.8 Barium Chloride—Soluble barium salts are poisonous
with Test Method D 2372. Retain the vehicle so obtained for
when taken by mouth. Read the appropriate MSDS before
use in the unsaponifiable matter (see 12.1) and fatty acids (see
using.
13.1) determinations.
5. Preparation of Sample
12. Unsaponifiable Matter
5.1 Onreceiptofasample,makearecordofthelabelnoting
12.1 Determine the unsaponifiable content of the vehicle in
especially the brand, the name of the manufacturer, and any
accordance with Test Method D 1398.
statement as to the composition of the paint and the net
contents. Weigh the unbroken package, open, note odor and
13. Fatty Acids
condition of the contents, pour into a clean container, and mix
13.1 Determine the fatty acids in accordance with Test
thoroughly by pouring from one container to the other, finally
Method D 1398.
leaving the well-mixed sample in the second container which
shall be tightly closed. The well-mixed sample shall be used at
14. Iodine Number of Fatty Acids
once for the analysis. The original can and cover may be
14.1 Determine the iodine number of fatty acids (see 13.1)
cleaned with a suitable solvent, wiped dry, and then weighed.
in accordance with Test Method D 1959.
This weight subtracted from the original weight will give the
net weight of the contents. If desired, the specific gravity of the
NOTE 1—If appreciable amounts of rosin or of unsaponifiable matter
paint may be determined, the weight per gallon calculated, and
are found to be absent in the vehicle of a paint, the iodine number of the
the volume of paint and the capacity of the container may be fatty acids gives the best indication (though not proof) of the presence of
linseed oil.An iodine number of less than 175 (Wijs) for the fatty acids is
measured.
an indication that the nonvolatile vehicle was not pure linseed oil.
15. Rosin
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
15.1 Determine the presence of rosin in the fatty acids (see
listed by the American Chemical Society, see Analar Standards for Laboratory
13.1) in accordance with Test Method D 1542.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
15.2 Ifdesired,determinetheamountofrosinquantitatively
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. in accordance with Test Method D 1469.
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.
D215–91 (2002)
ANALYSIS OF PIGMENT barium). The absence of calcium in this filtrate indicates that
Qualitative Analysis, Total Pigments—Single, Mixed, or the extending pigments contain no calcium carbonate (CaCO )
Composite or calcium sulfate (CaSO ); the absence of barium indicates
that the extending pigments contain no barium carbonate
16. Qualitative Analysis
(BaCO ).
16.1 Reagents:
NOTE 2—If the original sample contained BaCO , and lead sulfate
16.1.1 Acetic Acid.(Precaution—See 4.3)
(PbSO ), CaSO , or other soluble sulfate, the soluble barium will form
4 4
16.1.2 Acid Ammonium Acetate Solution—Mix 150 ml of
with the soluble sulfate a precipitate of BaSO which will be determined
acetic acid (8 + 2) 100 ml of water, and 95 ml of NH OH (sp
4 as“insolublematter.”Ifthesamplecontainedstrontiumsulfate(SrSO )or
gr 0.90).
strontium carbonate (SrCO ), some SrSO may be counted as BaSO ,
3 4 4
16.1.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated some strontium will count as soluble barium, and some may be counted as
calciumoxide(CaO).Strontiumisnotseparated,asitprobablywillnotbe
ammonium hydroxide (NH OH). (Precaution—See 4.1)
encountered, or will be present as an impurity in the barium and calcium
16.1.4 AmmoniumPolysulfide—PassH Sgasinto200mlof
compounds.
NH OH (sp gr 0.90) in a bottle immersed in running water or
in iced water until the gas is no longer absorbed; then add 200 16.2.2 Wash the matter insoluble in acid ammonium acetate
mL of NH OH (sp gr 0.90) and dilute with water to 1 litre. solution with another portion of this solution, and finally with
Digest this solution with 25 g of flowers of sulfur for several hot water. This insoluble matter shall be dried, ignited, and
hours and filter. testedforsiliceousmatter,BaSO ,andtitaniumcompounds.To
16.1.5 Ammonium Sulfate ((NH ) SO ). test for the latter, place a small amount of the insoluble matter,
4 2 4
16.1.6 Barium Chloride (BaCl ·2H O). (Precaution—See or of the original sample (about 0.5 g) in a 250-mL resistant
2 2
4.8) glass beaker; add 20 mL of concentrated H SO (sp gr 1.84)
2 4
16.1.7 Hydrochloric Acid (1+1)—Mix equal volumes of and 7 to 8 g of (NH ) SO . Mix well, and boil for a few
4 2 4
concentrated hydrochloric acid (HCl, sp gr 1.19) minutes. A residue denotes the presence of silica or siliceous
matter. Cool the solution, dilute with 100 mL of water, heat to
(Precaution—See 4.2) and water.
16.1.8 Hydrogen Peroxide (H O ), 3%. boiling, settle, filter, and wash with hot H SO (1 + 19) until
2 2 2 4
free from titanium.The residue may be tested for lead, barium,
16.1.9 Hydrogen Sulfide (H S). (Precaution—See 4.6)
16.1.10 Potassium Dichromate (K Cr O ). and silica.
2 2 7
16.1.11 Potassium Ferrocyanide, Standard Solution— 16.2.3 Add H O to a small portion of the filtrate; a clear
2 2
Dissolve 22 g of pure potassium ferrocyanide (K Fe(CN) · yellow-orange color indicates the presence of titanium. Boil
4 6
3H O)inwateranddiluteto1L.Tostandardize,transferabout another portion of the filtrate with metallic tin or zinc; a pale
0.2 g (accurately weighed) of pure metallic zinc or freshly blue to violet coloration indicates titanium.
ignited pure zinc oxide to a 400-mLbeaker. Dissolve in 10 mL 16.2.4 Treat another portion (about 1 g) of the pigment with
of HCl (sp gr 1.19) and 20 ml of water. Drop in a small piece 20mlofHCl(1 + 1)andnotewhetheranyH Sisevolved;boil
of litmus paper, add NH OH until slightly alkaline, add HCl the solution for about 5 min, add about 25 ml of hot water,
until just acid, and then 3 mL of HCl (sp gr 1.19). Dilute to filter, and wash with hot water. Render a small portion of the
about 250 mLwith hot water and heat nearly to boiling. Run in filtrate alkaline with NH OH, acidify with HCl, and add a little
the K Fe(CN) solution slowly from a buret, while stirring BaCl solution; a white precipitate (BaSO ) indicates the
4 6 2 4
constantly, until a drop tested on a white porcelain plate with a presence of a soluble sulfate. To another portion of the filtrate
drop of the uranyl indicator shows a brown tinge after standing add a little H SO ; a white precipitate indicates the presence of
2 4
1 min. A blank should be run with the same amounts of lead, soluble barium, or both (some CaSO may also separate).
reagents and water as in the standardization. The amount of Filter, wash to remove free acid, and treat the precipitate with
K Fe(CN) solutionrequiredfortheblankshouldbesubtracted a few drops of KI solution; the formation of yellow lead iodide
4 6
(PbI )indicatesthepresenceoflead.Thewhiteprecipitatemay
from the amounts used in standardization and in titration of the
sample. The standardization must be made under the same also be treated with H S water; the formation of black lead
sulfide (PbS) indicates the presence of lead.
conditions of temperature, volume, and acidity as obtained
when the sample is titrated. 16.2.5 To another portion of the original filtrate (see 16.2.1)
16.1.12 Potassium Iodide (KI). addNH OHuntilalkaline,renderslightlyacidwithaceticacid,
16.1.13 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric heat to boiling, and add a little K Cr O solution; a yellow or
2 2 7
acid (H SO ). (Precaution—See 4.2) orange-yellow precipitate indicates the presence of lead,
2 4
16.1.14 Sulfuric Acid (1+19)—Carefully mix 1 volume of soluble barium, or both. To another port
...