ASTM D283-13(2019)

Standard Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments

SIGNIFICANCE AND USE
3.1 This collection of test methods is used by pigment producers and paint manufacturers for process control, product acceptance, and research and development.
SCOPE
1.1 These test methods cover procedures for the chemical analysis of cuprous oxide and copper pigments.  
1.2 The analytical procedures appear in the following order:    
Sections  
Total Copper  
7  
Total Reducing Power as Cuprous Oxide  
8 and 9  
Metallic Copper  
10 and 11  
Cuprous Oxide  
12  
Cupric Oxide  
13  
Metals Other than Copper  
14 – 16  
Chlorides and Sulfates  
17 and 18  
Acetone-Soluble Matter  
19  
Water  
20  
Stability  
21  
Coarse Particles  
22  
Coarse Particles Insoluble in Nitric Acid  
23  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-May-2019
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.31 - Pigment Specifications

Relations

• Replaces: ASTM D283-13 - Standard Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments
• Effective Date: 01-Jun-2019
• Refers: ASTM D1208-96(2019) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 01-Jun-2019
• Refers: ASTM D1208-96(2012) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 01-Nov-2012
• Refers: ASTM D185-07 - Standard Test Methods for Coarse Particles in Pigments
• Effective Date: 01-Jul-2007
• Refers: ASTM D1208-96(2007) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 01-Jun-2007
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D185-84(1999) - Standard Test Methods for Coarse Particles in Pigments, Pastes, and Paints
• Effective Date: 10-May-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1208-96 - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 10-Nov-1996
• Refers: ASTM D1208-96(2002) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 10-Nov-1996
• Referred By: ASTM D964-03(2020) - Standard Specification for Metallic Copper Powder for Use in Antifouling Paints
• Effective Date: 01-Jun-2019

Overview

ASTM D283-13(2019): Standard Test Methods for Chemical Analysis of Cuprous Oxide and Copper Pigments establishes reliable laboratory procedures for determining the chemical composition of cuprous oxide and copper-based pigments. Developed by ASTM, this standard supports pigment producers and paint manufacturers in process control, product quality assurance, and research and development activities. Its globally recognized methodologies help ensure consistent pigment properties and regulatory compliance, critical in paint and coatings industries.

Key Topics

ASTM D283 describes step-by-step procedures and test methods to analyze essential pigment parameters, including:

• Total Copper Content - Determination of overall copper concentration in pigment samples.
• Total Reducing Power as Cuprous Oxide - Assessing the pigment’s reducing power expressed as cuprous oxide.
• Metallic Copper - Quantification of uncombined, metallic copper present in pigments.
• Cuprous Oxide and Cupric Oxide - Measuring the individual percentages of cuprous (Cu2O) and cupric oxide (CuO).
• Metals Other Than Copper - Identification and quantification of other metallic impurities, such as iron, cobalt, nickel, and zinc.
• Chlorides and Sulfates - Analysis of potentially harmful anions that may affect pigment stability or performance.
• Acetone-Soluble Matter and Water Content - Detection of residues and moisture affecting pigment usability and shelf life.
• Stability and Coarse Particles - Evaluating pigment stability under specific conditions and measuring particle size distribution, including those insoluble in nitric acid.

All test results are reported in SI units, aligning with international measurement standards.

Applications

These test methods bring practical value to a variety of industrial and research applications:

• Quality Control: Ensures pigment batches consistently meet product specifications by verifying chemical composition and purity.
• Product Acceptance: Provides a standardized basis for pigment approval in purchase and supply agreements within the paint and coatings industries.
• Research and Development: Facilitates formulation advances by enabling detailed studies of pigment properties and interactions.
• Regulatory Compliance: Assists manufacturers in meeting global regulatory requirements for pigments by documenting the presence and levels of specific chemical constituents.
• Process Optimization: Helps pigment producers refine manufacturing processes based on precise chemical analysis data.

By implementing ASTM D283 test methods, pigment manufacturers and paint formulators can minimize variability, improve end-product performance, and strengthen customer confidence.

Related Standards

For a comprehensive pigment quality program, ASTM D283 is frequently used with other relevant standards, including:

• ASTM D185 - Test Methods for Coarse Particles in Pigments: Used for particle size analysis.
• ASTM D1193 - Specification for Reagent Water: Prescribes water quality for analytic procedures.
• ASTM D1208 - Test Methods for Common Properties of Certain Pigments: For water content determination and other pigment properties.

These documents help laboratories implement robust, internationally aligned testing protocols for pigment evaluation.

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Keywords: ASTM D283, chemical analysis, cuprous oxide, copper pigments, pigment testing, paint manufacturing, quality control, pigment composition, pigment standards, international standard, copper oxide pigment analysis.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D283 − 13 (Reapproved 2019)
Standard Test Methods for
Chemical Analysis of Cuprous Oxide and Copper Pigments
This standard is issued under the fixed designation D283; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D1208 Test Methods for Common Properties of Certain
Pigments
1.1 These test methods cover procedures for the chemical
analysis of cuprous oxide and copper pigments.
3. Significance and Use
1.2 The analytical procedures appear in the following order:
3.1 This collection of test methods is used by pigment
Sections
producers and paint manufacturers for process control, product
Total Copper 7
acceptance, and research and development.
Total Reducing Power as Cuprous Oxide 8 and 9
Metallic Copper 10 and 11
4. Treatment of Sample
Cuprous Oxide 12
Cupric Oxide 13
4.1 Grind dry pigments, if lumpy or not finely ground, to a
Metals Other than Copper 14–16
Chlorides and Sulfates 17 and 18 fine powder and thoroughly mix (Note 1). Large samples may
Acetone-Soluble Matter 19
be thoroughly mixed and a representative portion taken and
Water 20
powderediflumpyornotfinelyground.Inallcasesthoroughly
Stability 21
Coarse Particles 22 mix the sample before taking portions for analysis. Preserve all
Coarse Particles Insoluble in Nitric Acid 23
samples in dry, dark, airtight and completely filled bottles or
1.3 The values stated in SI units are to be regarded as
containers to prevent oxidation. Some commercial copper
standard. No other units of measurement are included in this
oxides appear to segregate or oxidize rather easily. Therefore,
standard.
the thorough mixing of the sample to ensure homogeneity and
therapidhandlingofthesample,whenexposedtolightandair,
1.4 This standard does not purport to address all of the
are extremely important factors in obtaining accurate results
safety concerns, if any, associated with its use. It is the
NOTE 1—It is very important that the sample be thoroughly mixed.
responsibility of the user of this standard to establish appro-
Some samples of cuprous oxide are not homogeneous so are likely to give
priate safety, health, and environmental practices and deter-
trouble when an attempt is made to obtain concordant results. By placing
mine the applicability of regulatory limitations prior to use.
a few grams of a sample on a sheet of white paper and drawing it out with
1.5 This international standard was developed in accor- a spatula, it is frequently found that the sample contains coarse particles
of black scale, along with small balls of bright red cuprous oxide. Thus,
dance with internationally recognized principles on standard-
it may be necessary to pass the pigment through a No. 60 (250-µm) sieve,
ization established in the Decision on Principles for the
break up any lumps of ground pigment by gentle pressure, and grind any
Development of International Standards, Guides and Recom-
coarse particles failing to pass through the sieve. Since oxidation of slight
mendations issued by the World Trade Organization Technical
or even considerable magnitude may take place, these operations should
be performed quickly, avoiding prolonged grinding and exposure to light
Barriers to Trade (TBT) Committee.
and air.
2. Referenced Documents
5. Reagents
2.1 ASTM Standards:
5.1 Purity of Reagents—Reagent grade chemicals shall be
D185 Test Methods for Coarse Particles in Pigments
used in all tests. Unless otherwise indicated, it is intended that
D1193 Specification for Reagent Water
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
1 where such specifications are available. Other grades may be
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct used, provided it is first ascertained that the reagent is of
responsibility of Subcommittee D01.31 on Pigment Specifications.
Current edition approved June 1, 2019. Published June 2019. Originally
approved in 1928. Last previous edition approved in 2013 as D283 – 13. DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D0283-13R19. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D283 − 13 (2019)
sufficiently high purity to permit its use without lessening the 8.3 Ferrous Ammonium Sulfate, Standard Solution (0.03
accuracy of the determination. N)—Dissolve 12 g of ferrous ammonium sulfate
(Fe(NH ) (SO ) ·6H O) in 200 to 300 mL of water and add
4 2 4 2 2
5.2 Purity of Water—Unless otherwise indicated, references
40 mL of H SO (sp gr 1.84), while stirring constantly. Dilute
2 4
to water shall be understood to mean reagent water conforming
to 1 L in a volumetric flask. A few pieces of mossy aluminum
to Type II of Specification D1193.
may be added to stabilize the solution. The solution should be
5.3 Ammonium Sulfate—((NH ) SO ).
4 2 4 restandardized frequently against 0.1 N ceric ammonium ni-
trate solution.
5.4 Nitric Acid (sp gr 1.42)—Concentration nitric acid
(HNO
3).
8.4 Orthophenanthroline Indicator Solution (0.5 % in
water)—Orthophenanthroline ferrous complex (ferroin) shall
5.5 Perchloric Acid (70 %)—Concentrated perchloric acid
be used as the indicator.
(HClO ).
9. Procedure
6. Hazards
9.1 Weigh accurately (Note 2) 0.15 g of the sample and
6.1 Warning—Concentrated mineral acids cause burns of
place in a 250-mL, vented, glass-stoppered Erlenmeyer flask
the skin and eyes. Concentrated bases are also hazardous.
previously filled with carbon dioxide (CO ) or other inert gas.
Avoidcontactwithskinoreyes.Incaseofcontactimmediately 2
Addafewsmallglassbeadsand10mLofFeCI solution.Heat
flush skin or eyes with plenty of water. See appropriate MCA 3
gently for 15 min, stirring occasionally and maintaining at all
Safety Data Sheets for further information before handling
times an atmosphere of CO or other inert gas.
dangerous chemicals. 2
NOTE 2—The use of a 0.4-mLmicro beaker for weighing the specimen
6.2 Chemicals that have been declared toxic should be
is advised. The beaker is weighed first and the sample introduced into the
disposed of as hazardous chemicals and not discharged into a beaker, the correct weight obtained, and the entire beaker and its contents
dropped into the flask. This eliminates errors in weighing caused by
sink.
brushing the sample from glass balance pans.
TOTAL COPPER
9.2 After the specimen has been dissolved, cool, add 50 mL
of distilled water, and titrate at once with 0.1 N ceric ammo-
7. Procedure
nium nitrate solution until near the end point. Add 2 drops of
orthophenanthroline indicator solution and complete the titra-
7.1 Weigh accurately 1.0 g of the sample and transfer to a
tion. A sharp, distinct color change from orange to pale green
300-mL electrolytic beaker. Add 10 mL of concentrated nitric
occurs at the end point. Back-titrate with 0.03 N ferrous
acid (HNO ) and boil several minutes. Add 10 mL of HClO
3 4
ammonium sulfate solution to the orange color.
(70 %) and fume for 5 min. Cool, dilute to a volume of
approximately 150 mL, and add 1 mL of HNO and1gof
9.3 Calculation—Calculate the percent of total reducing
(NH ) SO .
4 2 4
power, A, as cuprous oxide (Cu O) as follows:
7.2 Carefully weigh the platinum electrode to 0.1 mg.
V N 2 V N 3 0.07154
1 1 2 2
A 5 3 100 (1)
Electroplate the copper on a rotating platinum electrode at a
S
current of 2 A for 2 h. Dilute with water and continue the
where:
electrolysis for 15 min. When the deposition is complete,
V = Ce(NH ) (NO ) solution required to titrate the
remove the electrode, wash with water and acetone, dry, and
1 4 2 3 6
specimen, mL,
weigh to 0.1 mg. Save the electrolyte for the determination of
N = normality of the Ce(NH ) (NO ) solution,
metals other than copper (Section 15).
1 4 2 3 6
V = Fe(NH ) (SO ) solution required for back-
2 4 2 4 2
7.3 Calculate the percent of total copper, Cu.
titration, mL,
N = normality of the Fe(NH ) (SO ) solution,
2 4 2 4 2
TOTAL REDUCING POWER AS CUPROUS OXIDE
S = specimen weight, g, and
0.07154 = equivalent weight of Cu O/1000.
8. Reagents
METALLIC COPPER
8.1 Ceric Ammonium Nitrate, Standard Solution (0.1 N)—
Mix 54.826 g of ceric ammonium nitrate (Ce(NH ) (NO ) )
4 2 3 6
10. Reagents
(either reagent grade or reference standard purity) with 56 mL
of sulfuric acid (H SO ) (1+1). Dissolve the salt and acid in
2 4 10.1 Ceric Ammonium Nitrate, Standard Solution (0.1 N)—
water, cool to room temperature, and dilute to 1 L. Standardize
See 8.1.
this solution against analyzed bright copper foil that has been
10.2 Denatured Alcohol (Formula No. 2B).
freed from all oxide coating.
8.2 Ferric Chloride Solution—Dissolve 75 g of ferric chlo-
ride (FeCI ·6H O) in a mixture of 150 mL of hydrochloric
3 2
This test method is based on the procedure described by Irvin Baker and R.
acid (HCl) (sp gr 1.19) and 400 mL of distilled water. Add 5
Stevens Gibbs, “Determination of Metallic Copper in Cuprous Oxide—Cupric
mL of hydrogen peroxide (H O ) (30 %) and boil to remove
2 2 Oxide Mixtures,” Industrial and Engineering Chemistry,Analytical Edition,Vol 13,
the excess. February 15, 1946, p. 124.
D283 − 13 (2019)
10.3 Extraction Solution—Add40mLofHCl(spgr1.19)to orthophenanthroline indicator solution. Titrate with 0.1 N ceric
1Lofdenaturedalcohol.Mixthoroughly.Add40gofstannous ammoniumnitratesolutionuntilthecolorchangesfromorange
chloride (SnCI ·2H O) and stir until completely dissolved. to pale green.
2 2
11.6 Calculation—Calculate the percent of metallic copper
10.4 Ferric Chloride Solution—See 8.2.
content, B, as follows:
10.5 Orthophenanthroline Indicatior—See 8.4.
V C
B 5 3 100 (2)
S
11. Procedure
where:
11.1 Add approximately 20 mL of 4-mm diameter glass
beads to a 250-mL Phillips beaker (assay flask). Weigh V = ceric ammonium nitrate solution required for titration
of the sample, mL,
accurately 0.15 g of sample on a tared, glazed paper approxi-
C = copper equivalent of the ceric ammonium nitrate
mately 13 mm square or a small watch glass that will fit into
solution, g/mL, and
the Phillips beaker, and transfer the specimen and paper or
S = specimen weight, g.
watch glass to the beaker. 2
11.2 Add 25 mL of denatured alcohol and swirl vigorously
CUPROUS OXIDE
for approximately 1 min to remove any surface coating and
12. Calculation
break up lumps. While swirling the flask, slowly add 100 mL
of the extraction solution.
12.1 Calculate the percent of cuprous oxide (Cu O), D,as
follows:
11.3 After the addition of the extraction solution, swirl the
flask vigorously for 5 min, adding lumps of dry ice (solid
D 5 A 2 2.252B (3)
carbondioxide)(Note3)continuouslyduringthistimetolower
whe
...