ASTM D3717-85a(2022)
(Test Method)Standard Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy
Standard Test Method for Low Concentrations of Antimony in Paint by Atomic Absorption Spectroscopy
SIGNIFICANCE AND USE
4.1 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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. Specific hazard statements are given in Section 7.
1.4 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
Relations
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: D3717 − 85a (Reapproved 2022)
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 with hydrochloric acid and stannous chloride. The antimony
content of the acid extract is determined by atomic absorption
1.1 This test method covers the determination of the content
spectroscopy.
of antimony in the range between 50 and 200 ppm (mg/kg)
present in the solids of liquid coatings or in dried films
4. Significance and Use
obtained from previously coated substrates. There is no reason
4.1 The permissible level of heavy metals in certain coat-
to believe that higher levels could not be determined by this
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
test method, provided that appropriate dilutions and adjust-
methodprovidesafullydocumentedprocedurefordetermining
ments in specimen size and reagent quantities are made.
low concentrations of antimony present in both water- and
1.2 The values stated in SI units are to be regarded as
solvent-reducible coatings to determine compliance.
standard. No other units of measurement are included in this
standard.
5. Apparatus
1.3 This standard does not purport to address all of the
5.1 Atomic Absorption Spectrophotometer, consisting of an
safety concerns, if any, associated with its use. It is the
atomizer and either a single- or three-slot burner; gas pressure
responsibility of the user of this standard to establish appro-
regulating and metering devices for air and acetylene; an
priate safety, health, and environmental practices and deter-
antimonysourcelampwitharegulatedconstantcurrentsupply;
mine the applicability of regulatory limitations prior to use.
a monochromator and associated optics; a photosensitive
Specific hazard statements are given in Section 7.
detector connected to an electronic amplifier; and a readout
1.4 This international standard was developed in accor-
device.
dance with internationally recognized principles on standard-
5.2 Muffle Furnace, maintained at 500 6 10 °C.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5.3 Oven, maintained at 105 6 2 °C.
mendations issued by the World Trade Organization Technical
5.4 Hot-Plate, with variable surface temperature control
Barriers to Trade (TBT) Committee.
over the range from 70 to 200 °C.
2. Referenced Documents
5.5 Reflux Condenser, water-cooled, and fitted with a
2.1 ASTM Standards: standard-taper joint.
D1193 Specification for Reagent Water
5.6 Erlenmeyer Flask, 125-mL, with standard-taper joint to
D2832 GuideforDeterminingVolatileandNonvolatileCon-
fit condenser.
tent of Paint and Related Coatings
5.7 Volumetric Flasks, 100 and 1000-mL.
3. Summary of Test Method
1 1
5.8 Dropping Bottles, 8 or 15-mL ( ⁄4 or ⁄2-oz) capacity.
3.1 The sample of liquid coating or dried film is prepared
5.9 Glass or Disposable Syringes, 10-mL capacity.
for analysis by dry ashing at 500 °C, followed by refluxing
5.10 Pipets, 1, 5, 10, and 15-mL capacity.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
5.11 Filter Paper, ashless, medium or slow filtering.
and Related Coatings, Materials, andApplications and is the direct responsibility of
5.12 Paint Shaker.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved June 1, 2022. Published June 2022. Originally
5.13 Paint Draw-Down Bar.
approved in 1978. Last previous edition approved in 2015 as D3717 – 85a (2015).
DOI: 10.1520/D3717-85AR22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Reagents
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. used in all tests. Unless otherwise indicated, it is intended that
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3717 − 85a (2022)
all reagents shall conform to the specifications of the Commit- 8.5 Aspirate the blank solution. When the recorder, meter,
tee onAnalytical Reagents of theAmerican Chemical Society, or other readout device reaches a constant value, it should be
where such specifications are available. Other grades may be immediately zeroed. Repeat this blank determination until a
used, provided it is first ascertained that the reagent is of steady, repeatable zero value is obtained at the maximum
sufficiently high purity to permit its use without lessening the response.
accuracy of the determination.
8.6 Aspirate each of the appropriate standard solutions in
6.2 Purity of Water—Unless otherwise indicated, references ascending antimony concentrations and record the correspond-
to water shall be understood to mean reagent grade water inginstrumentreadings.Aspiratewaterbetweeneachstandard.
conforming to Type II of Specification D1193.
NOTE 1—A deuterium background corrector, if available, should be
used to correct for background absorption. If not available, it is necessary
6.3 Antimony Standard Stock Solution (0.1 mg/mL)—
to reaspirate each standard solution and measure the background at a
Dissolve 0.1000 g of antimony metal in 40 mLof sulfuric acid
nearby nonabsorbing region of the spectrum.
(H SO , sp gr 1.84) by heating. Cool, carefully transfer
2 4
NOTE 2—Because of the high concentration and corrosive nature of the
quantitatively to a 1-L volumetric flask already approximately
acids used for the analysis, it is essential that the burner assembly be
half full with water, allow to cool to room temperature, and
disassembled and thoroughly cleaned out immediately after the analyses
are completed. Consult the instrument manual for cleaning instructions.
dilute to 1 L.
8.7 Construct a calibration curve on linear graph paper by
6.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
plotting the absorbance (corrected for background) versus
chloric acid (HCl).
concentration (micrograms per millilitre) for each standard
6.5 Stannous Chloride Solution (400 g/Lin HCl)—Dissolve
solution.
40 g of tin (II) chloride (SnCl ) in 50 mL of HCl (sp gr 1.19).
Transfer to a 100-mLvolumetric flask and fill to the mark with
9. Procedure
concentrated HCl.
9.1 If the sample is a liquid coating, mix it until
7. Hazards
homogeneous, preferably on a mechanical paint shaker. Deter-
mine the nonvolatile content in accordance with Guide D2832.
7.1 Use care in handling concentrated HCl because it is
corrosive and may cause burns to the skin and eyes and its
9.2 Prepare at least two replicate samples by weighing by
vapor is irritating to mucous membranes. Refer to suppliers’
difference from a dropping bottle or syringe, 5 to 10 g of the
Safety Data Sheet.
mixed liquid coating, or by directly weighing approximately 2
to6gof dried film, into 125-mL Erlenmeyer flasks. Weigh to
7.2 Use only a rubber bulb aspirator for pipetting liquids.
the nearest 0.1 mg.
8. Calibration and Standardization
NOTE 3—The specimen size called for will have a concentration of
8.1 Prepare 100-mL quantities of at least four standard
approximately 4 to 12 µg/mL antimony in the final diluted solution for
solutions brack
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