ASTM D3624-85a(2010)
(Test Method)Standard Test Method for Low Concentrations of Mercury in Paint by Atomic Absorption Spectroscopy
Standard Test Method for Low Concentrations of Mercury 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 mercury present in both water and solvent-reducible coatings to determine compliance.
SCOPE
1.1 This test method covers the determination of the content of mercury in the range between 10 and 1000 ppm (mg/kg) present in liquid coatings, coatings vehicles, 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 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 7 and 9.1.1.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3624 − 85a(Reapproved 2010)
Standard Test Method for
Low Concentrations of Mercury in Paint by Atomic
Absorption Spectroscopy
This standard is issued under the fixed designation D3624; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope methodprovidesafullydocumentedprocedurefordetermining
low concentrations of mercury present in both water and
1.1 This test method covers the determination of the content
solvent-reducible coatings to determine compliance.
of mercury in the range between 10 and 1000 ppm (mg/kg)
present in liquid coatings, coatings vehicles, or in dried films
5. Apparatus
obtained from previously coated substrates. There is no reason
to believe that higher levels could not be determined by this
5.1 Atomic Absorption Spectrophotometer—Any commer-
test method, provided that appropriate dilutions and adjust-
cial instrument having an open sample presentation area in
ments in specimen size and reagent quantities are made.
which to mount the absorption cell or an instrument designed
1.2 This standard does not purport to address all of the
specifically for the measurement of mercury using the cold
safety concerns, if any, associated with its use. It is the
vapor technique.
responsibility of the user of this standard to establish appro-
5.2 Recorder,0to10mV.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
5.3 Mercury Source Lamp.
statements are given in Section 7 and 9.1.1.
5.4 Absorption Cell—Standard spectrophotometer cells 100
2. Referenced Documents
mm long, having quartz end windows may be used. Prior to
2.1 ASTM Standards: use, the cell must be positioned in the optical path of the
D1193 Specification for Reagent Water
spectrophotometer and held in place by suitable clamps or
straps. The cell should be carefully aligned both vertically and
3. Summary of Test Method
horizontally to give the maximum transmittance.
3.1 The sample of liquid coating or dried film is weighed
5.5 Reduction Vessel—Cylindrical gas washing bottle, 250-
into a polytetrafluoroethylene (PTFE)-lined acid decomposi-
mL, equipped with a coarse (40 to 60-µm) fritted glass inlet
tion vessel and digested at an elevated temperature using
tube and a standard-taper glass stopper. Polyethylene or poly-
sulfuric and nitric acids. Use of a sealed acid decomposition
(vinyl chloride) tubing may be used for connecting the reduc-
vessel prevents loss of mercury during the digestion. The
tion vessel to the absorption cell.
digested sample is diluted to a known volume with water and
the concentration of mercury is determined using a cold-vapor,
5.6 Flowmeter, capable of measuring a gas flow of 1 L/min.
atomic absorption technique.
5.7 Drying Tube—Approximately 150 by 20-mm (6 by
4. Significance and Use
⁄4-in.) glass tube filled with magnesium perchlorate. The tube
4.1 The permissible level of heavy metals in certain coat-
should be filled each day that it is in use, and the Mg(ClO )
4 2
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
should be replaced whenever it becomes saturated (carefully
observe after each analysis).
This test method is under the jurisdiction of ASTM Committee D01 on Paint
NOTE 1—Use of an indicator desiccant at the exit end of the tube will
and Related Coatings, Materials, andApplications and is the direct responsibility of
make this observation easier.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved June 1, 2010. Published June 2010. Originally
5.8 Water Vapor Trap—A second 250-mL gas washing
approved in 1977. Last previous edition approved in 2005 as D3624 – 85a (2005).
DOI: 10.1520/D3624-85AR10.
bottle (the same as used for the reduction vessel). If preferred,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
a 250-mL Erlenmeyer vacuum flask fitted with a one-hole
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
stopper and 200 mm of 5-mm outside diameter glass tubing,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. may be substituted. (Fig. 1)
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3624 − 85a (2010)
FIG. 1 Apparatus
5.9 Mercury Trap—A 250-mL Erlenmeyer vacuum flask 6.4 Mercury Solution, Stock (1 mg/mL)—Dissolve 0.1354 g
containing 75 mL of 10 % sulfuric acid and 75 mL of 0.1 N of HgCl in 50 mL of water. Carefully add 5 mL of concen-
potassium permanganate solution to absorb the mercury vapor trated H SO and 3 mL of concentrated HNO and dilute to
2 4 3
after analysis. 100 mL. This solution contains 1000 µg/mL of mercury.
5.10 Circulating Oven, maintained at 140 6 5°C.
6.5 Mercury Standard, Working(0.1µg/mL)—Makesucces-
sivedilutionsofthestockmercurysolutiontoobtainaworking
5.11 Acid Decomposition Vessel, with 25-mL PTFE diges-
standard containing 0.1 mg/L (0.1 µg/mL), maintaining a
tion cup.
concentration of 5 % H SO and 3 % HNO by volume, in the
2 4 3
5.12 Volumetric Flasks, 100, 250, and 1000-mL.
diluted solutions. The working mercury standard and the
5.13 Paint Shaker. dilutions of the stock mercury solution should be prepared
fresh each day that it is used.
5.14 Paint Draw-Down Bar.
6.6 Nitric Acid(spgr1.42)Concentratednitricacid(HNO ).
6. Reagents
6.7 Nitrogen.
6.1 Purity of Reagents—Reagent grade chemicals shall be
6.8 Potassium Permanganate Solution (0.1 N)—Dissolve
used in all tests. Unless otherwise indicated, it is intended that
15.8 g of KMnO in water and dilute to 1 L.
all reagents shall conform to the specifications of the Commit-
6.9 Stannous Chloride Solution (100 g/L)Dissolve 25 g of
tee onAnalytical Reagents of theAmerican Chemical Society,
tin (II) chloride (SnCl ) by adding it to 60 mL of concentrated
where such specifications are available. Other grades may be 2
HCl (sp gr 1.19) and warming on a hotplate. When all of the
used, provided it is first ascertained that the reagent is of
SnCl has dissolved, transfer to a 250-mLvolumetric flask and
sufficiently high purity to permit its use without lessening the 2
dilute to volume with water. Mix well. This solution should be
accuracy of the determination.
prepared fresh each week that it is used.
6.2 Purity of Water—Unless otherwise indicated, references
6.10 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid
to water shall be understood to mean reagent water conforming
(H SO ).
to Type II of Specification D1193. 2 4
6.11 Sulfuric Acid (1+9)Carefully mix 1 volume of H SO
6.3 Hydroxylamine Hydrochloride Solution (100 g/L)— 2 4
(sp gr 1.84) into 9 volumes of water.
Dissolve 10 g of NH OH·HCl in 100 mL of water. Transfer a
portion of this solution to a small dropping bottle.
7. Hazards
7.1 Concentrated nitric and sulfuric acids are corrosive and
3 may cause severe burns of the skin or eyes. The vapor from
The sole source of supply of an acid decomposition vessel, Catalog No. 4745,
known to the committee at this time is the Parr Instrument Co., 211 Fifty-third St.,
concentratednitricacidisirritatingtomucousmembranes.Use
Moline, IL 61265. If you are aware of alternative suppliers, please provide this
care in handling these acidic substances. Refer to suppliers’
information to ASTM International Headquarters. Your comments will receive
1 Material Safety Data Sheet.
careful consideration at a meeting of the responsible technical committee, which
you may attend.
7.2 Mercury and its compounds are harmful and accumulate
Reagent Chemicals, American Chemical Society Specifications, American
in the aquatic environment. Mixtures containing mercury
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory compoundsshouldnotbeflusheddownadrain,butdisposedof
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
as hazardous waste.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. 7.3 Use only a rubber bulb aspirator for pipetting liquids.
D3624 − 85a (2010)
8. Calibration and Standardization 9. Procedure
9.1 If the sample is a liquid coating, mix it until
8.1 Assemble the various components, as illustrated in Fig.
homogeneous, preferably on a mechanical paint shaker. Pre-
1 if an atomic absorption spectrophotometer is used, or prepare
pare at least two replicate specimens by weighing to 0.1 mg by
the instrument for operation if a commercial mercury analyzer
difference from a dropping bottle or syringe, 100 to 200 mg of
is being used.
the mixed paint in
...
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