ASTM D3717-85a(2005)

Standard Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy

SIGNIFICANCE AND USE
The permissible level of heavy metals in certain coatings is specified by governmental regulatory agencies. This test method provides a fully documented procedure for determining low concentrations of antimony present in both water- and solvent-reducible coatings to determine compliance.
SCOPE
1.1 This test method covers the determination of the content of antimony in the range between 50 and 200 ppm (mg/kg) present in the solids of liquid coatings or in dried films obtained from previously coated substrates. There is no reason to believe that higher levels could not be determined by this test method, provided that appropriate dilutions and adjustments in specimen size and reagent quantities are made.
1.2 &si-value;
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. Specific hazard statements are given in Section .

General Information

• Status: Historical
• Publication Date: 31-Dec-2004
• 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 D3717-85a(1999) - Standard Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy
• Effective Date: 01-Jan-2005
• Replaced By: ASTM D3717-85a(2010) - Standard Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy
• Effective Date: 01-Jun-2010

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3717–85a(Reapproved2005)
Standard Test Method for
Low Concentrations of Antimony in Paint by Atomic
Absorption Spectroscopy
This standard is issued under the fixed designation D3717; 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 methodprovidesafullydocumentedprocedurefordetermining
low concentrations of antimony present in both water- and
1.1 This test method covers the determination of the content
solvent-reducible coatings to determine compliance.
of antimony in the range between 50 and 200 ppm (mg/kg)
present in the solids of liquid coatings or in dried films
5. Apparatus
obtained from previously coated substrates. There is no reason
5.1 Atomic Absorption Spectrophotometer, consisting of an
to believe that higher levels could not be determined by this
atomizer and either a single- or three-slot burner; gas pressure
test method, provided that appropriate dilutions and adjust-
regulating and metering devices for air and acetylene; an
ments in specimen size and reagent quantities are made.
antimonysourcelampwitharegulatedconstantcurrentsupply;
1.2 The values stated in SI units are to be regarded as
a monochromator and associated optics; a photosensitive
standard. No other units of measurement are included in this
detector connected to an electronic amplifier; and a readout
standard.
device.
1.3 This standard does not purport to address all of the
5.2 Muffle Furnace, maintained at 500 6 10°C.
safety concerns, if any, associated with its use. It is the
5.3 Oven, maintained at 105 6 2°C.
responsibility of the user of this standard to establish appro-
5.4 Hot-Plate, with variable surface temperature control
priate safety and health practices and determine the applica-
over the range from 70 to 200°C.
bility of regulatory limitations prior to use. Specific hazard
5.5 Reflux Condenser, water-cooled, and fitted with a
statements are given in Section 7.
standard-taper joint.
2. Referenced Documents 5.6 Erlenmeyer Flask, 125-mL, with standard-taper joint to
fit condenser.
2.1 ASTM Standards:
5.7 Volumetric Flasks, 100 and 1000-mL.
D1193 Specification for Reagent Water
1 1
5.8 Dropping Bottles, 8 or 15-mL ( ⁄4 or ⁄2-oz) capacity.
D2832 Guide for Determining Volatile and Nonvolatile
5.9 Glass or Disposable Syringes, 10-mL capacity.
Content of Paint and Related Coatings
5.10 Pipets, 1, 5, 10, and 15-mL capacity.
3. Summary of Test Method
5.11 Filter Paper, ashless, medium or slow filtering.
5.12 Paint Shaker.
3.1 The sample of liquid coating or dried film is prepared
5.13 Paint Draw-Down Bar.
for analysis by dry ashing at 500°C, followed by refluxing with
hydrochloric acid and stannous chloride.The antimony content
6. Reagents
of the acid extract is determined by atomic absorption spec-
6.1 Purity of Reagents—Reagent grade chemicals shall be
troscopy.
used in all tests. Unless otherwise indicated, it is intended that
4. Significance and Use
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
4.1 The permissible level of heavy metals in certain coat-
where such specifications are available. Other grades may be
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
This test method is under the jurisdiction of ASTM Committee D01 on Paint
accuracy of the determination.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Jan. 1, 2005. Published February 2005. Originally
approved in 1978. Last previous edition approved in 1999 as D3717 – 84 (1999). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D3717-85AR05. 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.
D3717–85a (2005)
are completed. Consult the instrument manual for cleaning instructions.
6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent grade water
8.7 Construct a calibration curve on linear graph paper by
conforming to Type II of Specification D1193.
plotting the absorbance (corrected for background) versus
6.3 Antimony Standard Stock Solution (0.1 mg/mL)—
concentration (micrograms per millilitre) for each standard
Dissolve 0.1000 g of antimony metal in 40 mLof sulfuric acid
solution.
(H SO , sp gr 1.84) by heating. Cool, carefully transfer
2 4
quantitatively to a 1-L volumetric flask already approximately
9. Procedure
half full with water, allow to cool to room temperature, and
9.1 If the sample is a liquid coating, mix it until homoge-
dilute to 1 L.
neous, preferably on a mechanical paint shaker. Determine the
6.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
nonvolatile content in accordance with Guide D2832.
chloric acid (HCl).
9.2 Prepare at least two replicate samples by weighing by
6.5 Stannous Chloride Solution (400 g/L in HCl)—Dissolve
difference from a dropping bottle or syringe, 5 to 10 g of the
40 g of tin (II) chloride (SnCl ) in 50 mL of HCl (sp gr 1.19).
mixed liquid coating, or by directly weighing approximately 2
Transfer to a 100-mLvolumetric flask and fill to the mark with
to6gof dried film, into 125-mL Erlenmeyer flasks. Weigh to
concentrated HCl.
the nearest 0.1 mg.
7. Hazards NOTE 3—The specimen size called for will have a concentration of
approximately 4 to 12 µg/mL antimony in the final diluted solution for
7.1 Use care in handling concentrated HCl because it is
paints containing approximately 200 ppm (mg/kg) antimony based on the
corrosive and may cause burns to the skin and eyes and its
nonvolatile content, and 1 to 3 µg/mLfor paints containing approximately
vapor is irritating to mucous membranes. Refer to suppliers’
50 ppm antimony, based on the nonvolatile content.
Material Safety Data Sheet.
NOTE 4—Recover dried paint films from previously coated substrates
(being careful not to remove any underlying material from the substrate)
7.2 Use only a rubber bulb aspirator for pipetting liquids.
or prepare in the laboratory from liquid samples. For the laboratory
preparation, flow some of the well-mixed sample onto a clean glass plate.
8. Calibration and Standardization
The use of a paint draw-down bar is recommended to obtain a uniform
8.1 Prepare 100-mL quantities of at least four standard
film thickness not exceeding 2 mils (50 µm). Allow the film to dry in an
solutions bracketing the expected antimony concentration in
oven at 1
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