ASTM D4358-84(1999)
(Test Method)Standard Test Method for Lead and Chromium in Air Particulate Filter Samples of Lead Chromate Type Pigment Dusts by Atomic Absorption Spectroscopy
Standard Test Method for Lead and Chromium in Air Particulate Filter Samples of Lead Chromate Type Pigment Dusts by Atomic Absorption Spectroscopy
SCOPE
1.1 This test method determines amounts of lead and chromium in residues obtained from air sampling of lead chromate and lead silico-chromate type pigment dusts. It is not applicable to all pigment dusts or to paint overspray samples of any kind.
1.2 This standard does not purport to address the safety problems 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.
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Designation:D4358–84 (Reapproved 1999)
Standard Test Method for
Lead and Chromium in Air Particulate Filter Samples of
Lead Chromate Type Pigment Dusts by Atomic Absorption
Spectroscopy
This standard is issued under the fixed designation D 4358; 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 hollow cathode source lamps with regulated constant current
supply; a monochromator with associated optics; a photode-
1.1 This test method determines amounts of lead and
tector; an amplifier; and digital or analog readout system.
chromium in residues obtained from air sampling of lead
5.2 Lead Hollow Cathode Lamp or electrodeless discharge
chromate and lead silico-chromate type pigment dusts. It is not
source lamp.
applicable to all pigment dusts or to paint overspray samples of
5.3 Chromium Hollow Cathode Source Lamp.
any kind.
5.4 Volumetric Flasks, 10-mL.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Reagents and Materials
responsibility of the user of this standard to establish appro-
6.1 Purity of Reagents—Reagent grade chemicals shall be
priate safety and health practices and determine the applica-
used in all tests. Unless otherwise indicated, it is intended that
bility of regulatory limitations prior to use.
all reagents shall conform to the Committee on Analytical
2. Referenced Documents Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, pro-
2.1 ASTM Standards:
vided it is first ascertained that the reagent is of sufficiently
D 1193 Specification for Reagent Water
high purity to permit its use without lessening the accuracy of
3. Summary of Test Method the determination.
6.2 Purity of Water—Unless otherwise indicated, references
3.1 The filter containing the air particulate sample is dis-
to water shall be understood to mean reagent water conforming
solved with nitric acid followed by treatment with 50 %
to Type II of Specification D 1193.
aqueous ammonium acetate solution. The solution is trans-
6.3 Ammonium Acetate Solution (50 % W/V aqueous)—
ferred to a volumetric flask and lead and chromium determined
Dissolve 250 g of ammonium acetate (NH C H O ) in water
by atomic absorption. 4 2 3 2
and dilute to 500 mL.
4. Significance and Use
6.4 Nitric Acid (sp gr 1.50)—Concentrated nitric acid
(HNO ).
4.1 This test method covers only the analysis of the pigment 3
6.5 Nitric Acid, (1 + 3)—Dilute 1 part concentrated nitric
dusts on filters, the results being expressed as micrograms of
acid with 3 parts water.
lead and of chromium. Sampling procedures are not a part of
6.6 Lead, Standard Stock Solution (1000 µg/mL)—Dissolve
this test method, nor are those calculations that are required to
0.1599 g of lead nitrate (Pb(NO ) ) in 50 mL of water
convert the results to concentration of lead and chromium in 3 2
containing 20 mL of concentrated HNO and 10 mL of 50 %
the sampled air, as required by the U.S. Occupational Safety
ammonium acetate solution, and dilute to 100 mL with water.
and Health Act (OSHA).
6.7 Chromium, Standard Stock Solution (1000 µg/mL)—
5. Apparatus
Dissolve 0.3734 g of potassium chromate (K CrO)in50mL
2 4
water containing 5 mLof concentrated HNO and dilute to 100
5.1 Atomic Absorption Spectrophotometer, consisting of an 3
mL with water.
atomizer and burner; gas pressure regulating and metering
devices for air, acetylene, and nitrous oxide; provision for
Reagent Chemicals, American Chemical Society Specifications, American
This test method is under the jurisdiction of ASTM Committee D-1 on Paint Chemical Society, Washington, DC. For suggestions on the testing of reagents not
and Related Coatings, Materials, andApplications and is the direct responsibility of listed by the American Chemical Society, see Analar Standards for Laboratory
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved April 27, 1984. Published August 1984. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4358
well as SO 5 interference may be reduced by adding 10 % of W/V
6.8 Filter Blank—Millipore 0.8-µm pore size, 37-mm diam-
KHSO to both standard and sample solution, employing an air/acetylene
eter, mixed esters of cellulose, Type AA white, plain, or
flame. The comparison of the experimental lead to chromium ratio noted
equivalent.
can be of some use here. (See Section 11.)
6.9 Hydrogen Peroxide—30 % (H O ).
2 2
7.12 Aspirate water into the flame. Then aspirate the 2.0
7. Calibration and Standardization
ppmstandardandadjustburnerpositionandflamecomposition
7.1 Good atomic absorption practice requires that the test
to give maximum absorption.
solutions being analyzed be aspirated into the flame inter-
7.13 Aspirate all standards into the flame, aspirating water
spersed between or at least contiguous to aspiration of the
between each standard and the next. Construct a calibration
calibration standards. The formal separation of calibration and
curve for chromium on linear graph paper by plotting the
analysis is for clarity of the methodology only and such
absorbanceversusconcentration(microgramspermillilitre)for
separation should not be made in practice.
each standard solution.
7.2 Operational instructions for atomic absorption spectro-
photometers vary with different models. Consult the manufac-
8. Procedure
turer’s literature for establishing optimum conditions for the
8.1 With each batch of samples a filter blank (minimum of
specific instrument used.
1 filter blank for every 10 filter samples) from the same
7.3 Insert the lead source lamp into the appropriate holder.
membrane lot must be analyzed. The filter blank is carried
Turn on the instrument and apply the current recommended by
through all steps of the analysis along with the sample(s).
the manufacturer to the source lamp. Allow the lead source
lampa10-minwarmup.Adjustthewavelengthto283.3nm,set 8.2 Carefully open the filter cassette containing the air
the slit to 0.7-nm bandpass, and maximize the transmitted
particulate sample. Remove the filter using forceps and deposit
energy by fine adjustment of the wavelength. it in a 50-mL beaker.
7.4 Prepare fresh standard solutions each day containing
8.3 Add6mLof1 + 3HNO ,coverthebeakerwithawatch
0.5, 1.0, 2.0, 5.0, and 10.0 ppm lead by appropriate dilutions of
glass, and keep just under boiling by placing on a hot water
the 1000 µg/mL stock standard. 20 mL of concentrated HNO
bath. Heat for 10 min. Add 2 mL of 50 % ammonium acetate
and 2 mL of 50 % ammonium acetate should be added in each
solution and continue to heat, adding water as needed to keep
case per 100 mL of final dilution.
the volume at about 5 to 6 mL. The solution must not be
7.5 Adjust the air and acetylene pressure or flow rates and
allowed to go to dryness. When analyzing lead silicochromate-
ignite the burner according to the instruction manual. Adjust
type pigment dusts, add 0.5 mL of 30 % hydrogen peroxide
the acetylene to give a rich flame. Allow a few minutes to
(H O ) after the 2 mLof 50 % ammonium acetate solution and
2 2
equilibrate.
continue heating until cellulose filter completely dissolves.
7.6 Aspirate water to rinse the atomizer chamber. Aspirate
8.4 Continue heating for 1 h. If the cellulose filter is not
the 10 ppm standard and make any necessary readjustment in
dissolved, continue the digestion until the solution is clear.
instrument parameters to obtain maximum absorption.
Cool and transfer to a 10.0-mL volumetric flask. Dilute to
7.7 Aspirate each standard solution and record the corre-
volume with water and determine lead and chromium.
sponding instrument readings. Aspirate 1 + 3 HNO , then
8.5 Prepare the atomic absorption instrument for lead as
water between each standard.
noted in 7.3, 7.5, and 7.6.
7.8 Constr
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