ASTM D3624-85a(1999)
(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
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 problems, 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.
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Designation:D3624–85a(Reapproved1999)
Standard Test Method for
Low Concentrations of Mercury in Paint by Atomic
Absorption Spectroscopy
This standard is issued under the fixed designation D 3624; 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.
1. Scope low concentrations of mercury present in both water and
solvent-reducible coatings to determine compliance.
1.1 This test method covers the determination of the content
of mercury in the range between 10 and 1000 ppm (mg/kg)
5. Apparatus
present in liquid coatings, coatings vehicles, or in dried films
5.1 Atomic Absorption Spectrophotometer—Any commer-
obtained from previously coated substrates. There is no reason
cial instrument having an open sample presentation area in
to believe that higher levels could not be determined by this
which to mount the absorption cell or an instrument designed
test method, provided that appropriate dilutions and adjust-
specifically for the measurement of mercury using the cold
ments in specimen size and reagent quantities are made.
vapor technique.
1.2 This standard does not purport to address all of the
5.2 Recorder,0to10mV.
safety concerns, if any, associated with its use. It is the
5.3 Mercury Source Lamp.
responsibility of the user of this standard to establish appro-
5.4 Absorption Cell—Standard spectrophotometer cells 100
priate safety and health practices and determine the applica-
mm long, having quartz end windows may be used. Prior to
bility of regulatory limitations prior to use. Specific hazard
use, the cell must be positioned in the optical path of the
statements are given in Section 7 and 9.1.1.
spectrophotometer and held in place by suitable clamps or
2. Referenced Documents straps. The cell should be carefully aligned both vertically and
horizontally to give the maximum transmittance.
2.1 ASTM Standards:
5.5 Reduction Vessel—Cylindrical gas washing bottle, 250-
D 1193 Specification for Reagent Water
mL, equipped with a coarse (40 to 60-µm) fritted glass inlet
3. Summary of Test Method
tube and a standard-taper glass stopper. Polyethylene or poly-
(vinyl chloride) tubing may be used for connecting the reduc-
3.1 The sample of liquid coating or dried film is weighed
tion vessel to the absorption cell.
into a polytetrafluoroethylene (PTFE)-lined acid decomposi-
5.6 Flowmeter, capable of measuring a gas flow of 1 L/min.
tion vessel and digested at an elevated temperature using
5.7 Drying Tube—Approximately 6 by ⁄4-in. (150 by 20-
sulfuric and nitric acids. Use of a sealed acid decomposition
mm) glass tube filled with magnesium perchlorate. The tube
vessel prevents loss of mercury during the digestion. The
should be filled each day that it is in use, and the Mg(ClO )
digested sample is diluted to a known volume with water and 4 2
should be replaced whenever it becomes saturated (carefully
the concentration of mercury is determined using a cold-vapor,
observe after each analysis).
atomic absorption technique.
NOTE 1—Use of an indicator desiccant at the exit end of the tube will
4. Significance and Use
make this observation easier.
4.1 The permissible level of heavy metals in certain coat-
5.8 Water Vapor Trap—A second 250-mL gas washing
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
bottle (the same as used for the reduction vessel). If preferred,
methodprovidesafullydocumentedprocedurefordetermining
a 250-mL Erlenmeyer vacuum flask fitted with a one-hole
stopper and 200 mm of 5-mm outside diameter glass tubing,
1 may be substituted.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
5.9 Mercury Trap—A 250-mL Erlenmeyer vacuum flask
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
containing 75 mL of 10 % sulfuric acid and 75 mL of 0.1 N
Current edition approved July 17 and Nov. 29, 1985. Published January 1986.
potassium permanganate solution to absorb the mercury vapor
Originally published as D 3624 – 77. Last previous edition D 3624 – 84.
after analysis.
Annual Book of ASTM Standards, Vol 11.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3624–85a (1999)
FIG. 1 Apparatus
5.10 Circulating Oven, maintained at 140 6 5°C. dilutions of the stock mercury solution should be prepared
5.11 Acid Decomposition Vessel, with 25-mL PTFE diges- fresh each day that it is used.
tion cup. 6.6 Nitric Acid (sp gr 1.42) Concentrated nitric acid
5.12 Volumetric Flasks, 100, 250, and 1000-mL. (HNO ).
5.13 Paint Shaker. 6.7 Nitrogen.
5.14 Paint Draw-Down Bar. 6.8 Potassium Permanganate Solution (0.1 N)—Dissolve
15.8 g of KMnO in water and dilute to 1 L.
6. Reagents
6.9 Stannous Chloride Solution (100 g/L) Dissolve 25 g of
tin (II) chloride (SnCl ) by adding it to 60 mL of concentrated
6.1 Purity of Reagents—Reagent grade chemicals shall be 2
HCl (sp gr 1.19) and warming on a hotplate. When all of the
used in all tests. Unless otherwise indicated, it is intended that
SnCl has dissolved, transfer to a 250-mLvolumetric flask and
all reagents shall conform to the specifications of the Commit- 2
dilute to volume with water. Mix well. This solution should be
tee onAnalytical Reagents of theAmerican Chemical Society,
prepared fresh each week that it is used.
where such specifications are available. Other grades may be
6.10 Sulfuric Acid (sp gr 1.84) Concentrated sulfuric acid
used, provided it is first ascertained that the reagent is of
(H SO ).
sufficiently high purity to permit its use without lessening the 2 4
6.11 Sulfuric Acid (1+9) Carefully mix 1 volume of
accuracy of the determination.
H SO (sp gr 1.84) into 9 volumes of water.
6.2 Purity of Water—Unless otherwise indicated, references 2 4
to water shall be understood to mean reagent water conforming
7. Hazards
to Type II of Specification D 1193.
7.1 Concentrated nitric and sulfuric acids are corrosive and
6.3 Hydroxylamine Hydrochloride Solution (100 g/L)—
may cause severe burns of the skin or eyes. The vapor from
Dissolve 10 g of NH OH·HCl in 100 mL of water. Transfer a
concentratednitricacidisirritatingtomucousmembranes.Use
portion of this solution to a small dropping bottle.
care in handling these acidic substances. Refer to suppliers’
6.4 Mercury Solution, Stock (1 mg/mL)—Dissolve 0.1354 g
Material Safety Data Sheet.
of HgCl in 50 mL of water. Carefully add 5 mL of concen-
7.2 Mercury and its compounds are harmful and accumulate
trated H SO and 3 mL of concentrated HNO and dilute to
2 4 3
in the aquatic environment. Mixtures containing mercury
100 mL. This solution contains 1000 µg/mL of mercury.
compoundsshouldnotbeflusheddownadrain,butdisposedof
6.5 Mercury Standard, Working (0.1 µg/mL)—Makesucces-
as hazardous waste.
sivedilutionsofthestockmercurysolutiontoobtainaworking
7.3 Use only a rubber bulb aspirator for pipetting liquids.
standard containing 0.1 mg/L (0.1 µg/mL), maintaining a
concentration of 5 % H SO and 3 % HNO by volume, in the
2 4 3
8. Calibration and Standardization
diluted solutions. The working mercury standard and the
8.1 Assemble the various components, as illustrated in Fig.
1 if an atomic absorption spectrophotometer is used, or prepare
the instrument for operation if a commercial mercury analyzer
The sole source of supply of an acid decomposition vessel, Catalog No. 4745,
is being used.
known to the committee at this time is the Parr Instrument Co., 211 Fifty-third St.,
Moline, IL 61265. If you are aware of alternative suppliers, please provide this
NOTE 2—Be sure that all glassware has been thoroughly cleaned and
information to ASTM Headquarters. Your comments will receive careful consider-
rinsed with reagent water prior to use.
ation at a meeting of the responsible technical committtee, which you may attend
8.2 Operational instructions for atomic absorption spectro-
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
photometers and commercial mercury analyzers vary with
listed by the American Chemical Society, see Analar Standards for Laboratory
different models. Consult the manufacturer’s literature for
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
establishing optimum conditions for the specific instrument
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. used.
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