ASTM D1135-86(2004)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D1135–86(Reapproved2004)
Standard Test Methods for
Chemical Analysis of Blue Pigments
This standard is issued under the fixed designation D 1135; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 2. Referenced Documents
1.1 These test methods cover procedures for the chemical 2.1 ASTM Standards:
analysis of blue pigments known commercially as iron blue, D 280 Test Methods for Hygroscopic Moisture (and Other
copper phthalocyanine blue, and ultramarine blue. Matter Volatile Under the Test Conditions) in Pigments
1.2 The analytical procedures appear in the following order: D 1193 Specification for Reagent Water
D 1208 Test Methods for Common Properties of Certain
Sections
Pigments
IRON BLUE PIGMENTS
D 2448 TestMethodforWater-SolubleSaltsinPigmentsby
Measuring the Specific Resistance of the Leachate of the
Identification 6
Moisture by the Brabender Moisture Tester 7 and 8
Pigment
Moisture by Toluene Distillation 9
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
Water-Soluble Matter by Extraction 10
poses
Water-Soluble Salts by Electrical Conductivity 11
Detection of Acid-Insoluble Extenders 1213
Detection of Acid-Soluble Extenders 14 to 17
3. Significance and Use
Detection of Organic Colors and Lakes 18
3.1 These test methods are suitable for determining if
COPPER PHTHALOCYANINE BLUE PIGMENTS
impurities are present and establishing that the required pig-
ments are present. These test methods may be used for
Identification 19
Moisture and Other Volatile Matter 20 manufacturing quality control.
Detection of Basic Dye Derivatives 21
Detection of Other Organic Coloring Matter 22
4. Purity of Reagents and Water
Detection of Ultramarine Blue 23
4.1 Purity of Reagents—Unless otherwise indicated, it is
Detection of Iron Blue 24
intended that all reagents shall conform to the specifications of
ULTRAMARINE BLUE
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
cal Society, where such specifications are available. Other
Identification 25
Moisture and Other Volatile Matter 26
grades may be used, provided it is first ascertained that the
Water-Soluble Matter 27
reagent is of sufficiently high purity to permit its use without
Detection of Basic Dye Derivatives 28
lessening the accuracy of the determination.
Detection of Other Organic Coloring Matter 29
1.3 This standard does not purport to address the safety
concerns associated with its use. It is the responsibility of the
user of this standard to establish appropriate safety and health
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
practices and determine the applicability of regulatory limita-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tions prior to use.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Reagent Chemicals, American Chemical Society Specifications, American
These test methods are under the jurisdiction of ASTM Committee D01 on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Paint and Related Coatings, Materials, and Applications and are the direct listed by the American Chemical Society, see Analar Standards for Laboratory
responsibility of Subcommittee D01.31 on Pigment Specifications. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved June 1, 2004. Published June 2004. Originally and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
approved in 1950. Last previous edition approved in 1999 as D 1135 – 86 (1999). MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1135–86 (2004)
4.2 Purity of Water—Unless otherwise indicated, references 5.2 Grind extracted pigments to pass a No. 80 (180-µm)
towatershallbeunderstoodtomeanreagentwaterconforming sieve. Discard any skins that do not pass through the sieve.
to Type II of Specification D 1193.
Mix the finely ground pigment thoroughly.
5. Preparation of Sample
5.1 Mix the sample thoroughly and take a representative
portion for analysis. Reduce any lumps or coarse particles to a
fine powder by grinding. Detailed requirements for this sieve are given in Specification E 11.
IRON BLUE
(Prussian Blue, Chinese Blue, Milori Blue)
door must not be opened.
IDENTIFICATION
8.3 Calculation and Report—Plot time against percent loss
6. Procedure
in weight on rectilinear cross-section paper. Extrapolate the
6.1 To approximately 0.1 g of pigment in a 50-mL beaker, linear portion of the curve to zero time. That portion beyond
add15mLofNaOHsolution(50g/L).Heattoboiling.Inafew about 2 h will be essentially linear. Report the percent loss in
minutes the blue color should be completely destroyed, giving weight at the extrapolated zero time as the percent moisture in
initsplacethecharacteristicreddishbrownprecipitateofferric the pigment.
hydroxide.Add HCl (1+1) until faintly acid to litmus.The iron
NOTE 3—The pigment undergoes a slight loss in weight due to
blue should be reformed, yielding again the characteristic blue
decomposition during the heating. The method of plotting and extrapola-
color.
tion corrects for this loss.An approximate value for moisture content may
be obtained by taking the reading at the end of the first hour’s heating.An
NOTE 1—If the NaOH treatment does not completely destroy the blue
occasional pigment may decompose rapidly at the oven temperature. In
color, the evidence is strong that a foreign pigment is present. If this
such cases, determine moisture by the toluene distillation method (Section
occurs, it is best to filter the alkaline solution, weakly acidify the filtrate
9).
with HCl (1+1), and add approximately 2 mL of a ferric salt solution
(ferric sulfate or ferric alum (20 g/L)). The formation of a blue precipitate
MOISTURE BY TOLUENE DISTILLATION
established the pigment as consisting, at least in part, of iron blue.
9. Procedure
MOISTURE BY THE BRABENDER MOISTURE
TESTER
9.1 Determine the moisture content in accordance with
Sections 7 and 8 of Test Method D 1208, but using 25 g of
7. Apparatus
pigment and 200 mL of toluene and adjusting the calculation
accordingly.
7.1 Brabender Moisture Tester—The Brabender moisture
tester (Fig. 1) consists of a constant-temperature oven with
WATER-SOLUBLE MATTER BY EXTRACTION
weighing apparatus attached. Specimens placed in the oven
may be weighed without opening the oven door or removing
10. Procedure
the specimen from the oven, as the balance scale is calibrated
10.1 Determine whether or not the pigment is easily wet by
to read directly in percent of moisture.
water at room temperature by adding a little to some water in
8. Procedure a beaker. If it tends to float on top of the water with very little,
if any, tendency to sink to the bottom or disperse throughout
8.1 Set the temperature control at 160°C and allow the oven
the solution, even after agitation, it contains a hydrophobic
to reach this temperature before checking or making any
treating agent.
weighing. Check the scale by placing a sample dish containing
10.2 Weigh to 1 mg about 2.5 g of the pigment into a
9.200 g standard analytical balance weights in the oven. The
250-mL volumetric flask. If the pigment is hydrophobic as
apparatus should read 8.0 % moisture. If it does not, adjust to
tested above, moisten thoroughly with a few mL of ethyl
a reading of 8.0 % by turning either the right hand or left hand
alcohol (Note 4). If the pigment is easily wet with water, no
foot screw.
alcohol is necessary. Fill the flask about half full with water
8.2 Weigh 10.000 g of the sample into the aluminum dish
and shake to disperse the pigment thoroughly. Fill to the mark
and place in the oven. For a series of specimens, all should be
and again shake. Allow to remain at room temperature for not
placed in the oven at as nearly the same time as possible. No
less than 15 h, shaking from time to time, preferably with an
specimen should occupy the position directly in front of the
automatic shaking device.
door.Weigh the specimen at the end of each hour for 5 h.After
each weighing, return the specimen to its original place in the
NOTE 4—Ethyl alcohol denatured with acetone (Formula No. 23A) or
oven. denatured with methyl alcohol (Formula No. 3A) has been found suitable.
10.3 Let settle, filter through a dry filter paper, and discard
NOTE 2—The dried pigment is very hygroscopic. In order to obtain
consistentresults,thespecimenpositionmustnotbechangedandtheoven the first 20 mL of the filtrate. Transfer 100 mL of the clear
D1135–86 (2004)
FIG. 1 Brabender Moisture Tester
filtrate to a weighed dish, and evaporate to dryness on a steam pigment but not high enough to render the iron difficultly
bath. Dry for1hinan oven at 105 6 2°C, cool, and weigh. soluble in HCl (Note 5). Cool, and add 15 mL of HCl (sp gr
10.4 Calculation—Calculate the percent of water-soluble 1.19) and a few drops of bromine. Cover with a watch glass
matter as follows: and evaporate to a sirup. Add about 15 mL of water, and boil.
It may be necessary to add a drop or two of HCl to effect
Water2soluble matter, % 5 grams of residue 3 100
complete solution of the ferric iron residue. Filter and wash
WATER-SOLUBLE SALTS BY ELECTRICAL
with hot water. Save the filtrate for the determination of
CONDUCTIVITY
alumina hydrate (Section 16).
11. Procedure NOTE 5—The ignition can conveniently be carried out in a 250-mL
beaker or a porcelain dish over a free flame. Oxidation of the specimen is
11.1 Determine water-soluble salt content in accordance
evidenced by a dull glowing.While being heated, it is advisable to roll the
with Test Method D 2448.
specimen around in the beaker or dish exposing all of the surface to the
oxygen of the air.Amoderately low flame should be used and the ignition
DETECTION OFACID-INSOLUBLE EXTENDERS
is complete when the specimen ceases to glow and acquires a uniform
brown color.
12. Scope
13.2 Aresidue of less than 3 mg that appears as small black
12.1 Acid-insolubleextendersincludebariumsulfate,silica,
specks can be neglected, since quite frequently a small amount
and silicates. Alumina may also be found, in part, with this
ofironisrenderedinsolubleorasmallamountofbluepigment
group.
escapes destruction. Ignite the residue and weigh. If apprecia-
13. Procedure
bly more than 3 mg are pre
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