ASTM C738-94(1999)
(Test Method)Standard Test Method for Lead and Cadmium Extracted from Glazed Ceramic Surfaces
Standard Test Method for Lead and Cadmium Extracted from Glazed Ceramic Surfaces
SCOPE
1.1 This test method covers the precise determination of lead and cadmium extracted by acetic acid from glazed ceramic surfaces. The procedure of extraction may be expected to accelerate the release of lead from the glaze and to serve, therefore, as a severe test that is unlikely to be matched under the actual conditions of usage of such ceramic ware. This test method is specific for lead and cadmium.
1.2 The values stated in SI (metric) units are to be regarded as the standard. The values given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:C738 – 94 (Reapproved 1999)
Standard Test Method for
Lead and Cadmium Extracted from Glazed Ceramic
Surfaces
This standard is issued under the fixed designation C 738; 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 ditions recommended by instrument manufacturer. Using these
conditions, characteristic concentration (concentration that
1.1 This test method covers the precise determination of
gives 0.0044 absorbance) should be approximately (620 %)
leadandcadmiumextractedbyaceticacidfromglazedceramic
0.2 and 0.45 ppm for Pb measured at 217.0 and 283.3 nm,
surfaces. The procedure of extraction may be expected to
respectively. Characteristic concentration should be approxi-
accelerate the release of lead from the glaze and to serve,
mately (620 %) 0.02 ppm for Cd.
therefore, as a severe test that is unlikely to be matched under
the actual conditions of usage of such ceramic ware. This test
NOTE 1—1 ppm = 1 µg/mL.
method is specific for lead and cadmium.
4.2 Lead Lamp, set at 283.3 or 217.0 nm.
1.2 The values stated in SI (metric) units are to be regarded
4.3 Cadmium Lamp, set at 228.8 nm.
as the standard. The values given in parentheses are for
4.4 Glassware of chemically resistant borosilicate glass, to
information only.
make reagents and solutions. Clean by rinsing with dilute nitric
1.3 This standard does not purport to address all of the
acid(10 %byvolume)followedbycopiousquantitiesofwater.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Reagents
priate safety and health practices and determine the applica-
5.1 Purity of Reagents—Reagent grade chemicals shall be
bility of regulatory limitations prior to use.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
2. Summary of Test Method
tee onAnalytical Reagents of theAmerican Chemical Society,
2.1 Lead and cadmium are extracted from the test article by
where such specifications are available. Other grades may be
leaching with 4 % acetic acid for 24 h at 20 to 24°C (68 to
used provided it is first ascertained that the reagent is of
75°F) and are measured by flame atomic absorption spectros-
sufficiently high purity to permit its use without lessening the
copy.
accuracy of the determination.
5.2 Purity of Water—Unless otherwise indicated, references
3. Interferences
to water shall be understood to mean distilled water.
3.1 There are no interferences when instrumental back-
5.3 Acetic Acid (4 % by Volume)—Mix 1 volume of glacial
ground correction and light sources specific for lead and
acetic acid with 24 volumes of water.
cadmium are used.
5.4 Detergent Wash—Use detergent designed for washing
household dishes by hand. Mix with lukewarm tap water
4. Apparatus
according to product instructions.
4.1 Atomic Absorption Spectrometer equipped with light
5.5 Lead Nitrate Solution (1000-ppm Pb)—Dissolve 1.598
sources (hollow cathode or electrodeless discharge lamps)
g of lead nitrate (Pb(NO ) ) in 4 % acetic acid and dilute to 1
3 2
specific for lead and cadmium, instrumental background cor-
L with 4 % acetic acid. Commercially available standard lead
rection,anda4-in.(102-mm)singleslotorBolingburnerhead.
solutions may also be used.
Digital concentration readout may be used. Use air-acetylene
5.6 Hydrochloric Acid (1 % by weight)—Mix 1 volume of
flame, instrumental background correction, and operating con-
concentrated hydrochloric acid (HCl, sp gr 1.19) with 37
volumes of water.
This test method is under the jurisdiction of ASTM Committee C-21 on
Ceramic Whitewares and Related Products and is the direct responsibility of
Subcommittee C21.03 on Test Methods for Whiteware Properties. This test method Reagent Chemicals, American Chemical Society Specifications, American
was developed jointly by theAOAC andASTM, and adopted official final action by Chemical Society, Washington, DC. For suggestions on the testing of reagents not
the Association of Official Analytical Chemists (method 973.32 AOAC Offıcial listed by the American Chemical Society, see Analar Standards for Laboratory
Methods of Analysis (1990) 15th ed, AOAC International, Arlington, VA. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved July 15, 1994. Published September 1994. Originally and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
published as C 738 – 72. Last previous edition C 738 – 94. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C738 – 94 (1999)
TABLE 1 Mean Value Required in a Large Lot for Failure Rate
5.7 Cadmium Solution (1000-ppm Cd)—Dissolve 0.9273 g
1/10000 with Coefficient of Variation 60%
ofanhydrouscadmiumsulfateinapproximately250mLof1 %
Worstof6
HCl (see 5.6) and dilute to 500 mL with 1 % HCl. Commer-
Limit (ppm) Mean of 6
(Mean of 1)
cially available standard cadmium solutions may also be used.
7 3.21 1.45
5 2.29 1.03
6. Procedure
2.5 1.15 0.52
NOTE 2—Take a method control through entire procedure. Use a 0.7 0.32 0.14
0.5 0.23 0.10
laboratory beaker with dimensions similar to ware being tested.
0.25 0.11 0.05
6.1 Preparation of Sample—Take, at random, six identical
units and the method control vesse
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