1、Designation: C895 87 (Reapproved 2014)Standard Test Method forLead and Cadmium Extracted from Glazed Ceramic Tile1This standard is issued under the fixed designation C895; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the precise determination oflead and cadmium extracted by acetic acid from glazed ceramictile
3、 that are intended for use in areas of food preparation. Theprocedure of extraction may be expected to accelerate therelease of lead from the glaze and to serve, therefore, as asevere test that is unlikely to be matched under the actualconditions of usage of such ceramic tile. This test method isspe
4、cific for lead and cadmium.1.2 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.3 This standard does not purport to address all of thesa
5、fety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C738 Test Method for Lead and
6、Cadmium Extracted fromGlazed Ceramic SurfacesC1034 Test Method for Lead and Cadmium Extracted FromGlazed Ceramic Cookware (Withdrawn 2001)3C1035 Specification for Lead and Cadmium Extracted fromGlazed Ceramic Cookware (Withdrawn 2001)33. Summary of Test Method3.1 The lead and cadmium extracted from
7、the article undertest, by acetic acid at 20 to 24C (68 to 75F) after 24 h ofleaching, are measured by atomic absorption spectrophotom-etry using specific hollow-cathode lamps for lead andcadmium, respectively.4. Significance and Use4.1 There are several test methods available to measure thelead and
8、cadmium release from dinnerware and cookware (seeTest Methods C738 and C1034 and Specification C1035).These standards are used as a control to ensure the protectionof the population against a possible health hazard.4Thispotential hazard arises with improperly formulated, applied,fired glazes and dec
9、orations. This test method deals specificallywith ceramic tile that are intended to come in contact with foodduring its preparation (for example, counter top tile).5. Interferences5.1 Since specific hollow-cathode lamps for lead and cad-mium are used, there are no interferences.6. Apparatus6.1 Atomi
10、c Absorption Spectrophotometer, equipped with a4-in. (102-mm) single slot or Boling burner head and digitalconcentration readout attachment (DCR) if available. Thisinstrument should have a sensitivity of about 0.5 ppm of leadfor 1 % absorption and a sensitivity of about 0.25 ppm ofcadmium for 1 % ab
11、sorption. Use the operating conditions asspecified in the instrument manufacturers analytical methodsmanual.NOTE 11 ppm = 1 mg/L or one part per million is one milligram perlitre.6.2 Hollow-Cathode Lead Lamp, with wavelength set at283.3 or 217.0 nm.6.3 Hollow-Cathode Cadmium Lamp, with wavelength se
12、tat 228.8 nm.6.4 Glassware of chemically resistant borosilicate glass tomake reagents and solutions.6.5 Test CellChemically resistant borosilicate glass cylin-der to contain the leaching solution. An open-ended cellapproximately 80 mm in length and 60 mm in internal diameterhas proven suitable.1This
13、 test method is under the jurisdiction ofASTM Committee C21 on CeramicWhitewares and Related Productsand is the direct responsibility of SubcommitteeC21.06 on Ceramic Tile.Current edition approved Dec. 1, 2014. Published December 2014. Originallyapproved in 1978. Last previous edition approved in 20
14、09 as C895 87 (2009).DOI: 10.1520/C0895-87R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last appro
15、ved version of this historical standard is referenced onwww.astm.org.4“Lead Industries, Inc.,” Proceedings, International Conference on CeramicFoodware Safety, 1975, pp. 817.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Reagents7
16、.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Societywhere such specifications are available.5Other grades may b
17、eused provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled water.7.3 Acetic Acid (4 % by Volume)Mix
18、1 volume of glacialacetic acid with 24 volumes of water. Run a reagent blank eachtime a 4 % acetic acid solution is prepared.7.4 Detergent RinseAdd 15 g of suitable alkaline deter-gent to 1 gal (3.79 L) of lukewarm tap water.7.5 Lead Nitrate Solution (1000-ppm Pb)Dissolve 1.598 gof lead nitrate (Pb(
19、No3)2) in 4 % acetic acid and dilute to 1 Lwith 4 % acetic acid. Commercially available standard leadsolutions may also be used.7.6 Hydrochloric Acid (1 % by Weight)Mix 1 volume ofconcentrated hydrochloric acid (HCl, sp. gr. 1.19) with 37volumes of water.7.7 Cadmium Solution (1000-ppm Cd)Dissolve 0.
20、9273 gof anhydrous cadmium sulfate in approximately 250 mLof 1 %HCl (see 7.6), and dilute to 500 mL with 1 % HCl. Commer-cially available standard cadmium solutions may also be used.8. Procedure8.1 Preparation of SampleTake, at random, six identicaltiles and cleanse the surface of each with a deterg
21、ent rinse.Then rinse with tap water, followed by distilled water, and dry.Using a suitable silicone rubber sealant free of lead andcadmium, seal the test cell to the glazed surface. Fill each cellwith sufficient 4 % acetic acid to achieve a ratio of 25 mL ofsolution to each 1 in.2(6.45 cm2) of expos
22、ed glaze surface.Record the volume of acid used in each cell. If the tile beingtested has a surface dimension less than 60 mm (smaller thanthe diameter of the test cell), a suitable number of tiles shall bemounted and grouted6to provide the required test area.Mounting, grouting, and grout cleanup sh
23、ould precede thedetergent rinse. Each mounted set constitutes one test sample.Cover each test with a glass plate to prevent evaporation ofsolution, avoiding contact between cover and surface ofleaching solution. The extraction shall be run in total darkness,and the test array must be covered with an
24、 opaque cloth or foilto prevent exposure to light. Let stand for 24 h at 20 to 24C(68 to 74F).8.2 Preparation of Standards:8.2.1 Lead StandardsDilute lead nitrate solution (see 7.5)with acetic acid (see 7.3) to obtain working standards havingfinal concentrations of 0, 5, 10, 15, and 20 ppm of Pb.8.2
25、.2 Cadmium StandardsDilute cadmium stock solution(see 7.7) with acetic acid (see 7.3) to obtain working standardshaving final concentrations of 0.0, 0.3, 0.5, 1, 1.5, and 2.0 ppmof Cd.8.3 Determination of Lead by Atomic AbsorptionStir thesample (leaching) solution and pour off a portion into a clean
26、flask. Using the atomic absorption spectrophotometer (see 6.1)and hollow-cathode lamp (see 6.2), at the same time determinethe absorption of the lead working standards (see 8.2.1) andsample (leaching) solutions, diluting the latter with 4 % aceticacid if required (if solution contains over 20 ppm).
27、Concentratesamples containing less than 1 ppm of lead by accuratelytransferring a minimum of 50.0 mL of solution to a 250-mLbeaker and evaporating to dryness on a steam bath. Dissolvethe residue in 4 % acetic acid by adding exactly 0.1 of thevolume of the solution taken for concentration, cover with
28、watch glass, and swirl to complete dissolution. Prepare astandard curve of absorption versus concentration (ppm).Determine the lead content (ppm Pb) of sample (leaching)solution from the standard curve. If digital concentrationreadout is used, the standard curve is not necessary. However,standards b
29、racketing the solution under test should be used.8.4 Determination of Cadmium by Atomic AbsorptionSpectrophotometryProceed as in 8.3 using the cadmiumhollow-cathode lamp (see 6.3) and cadmium standards (see8.2.2). If the sample (leaching) solutions contain more than 2ppm of Cd, dilute with 4 % aceti
30、c acid. Concentrate samplescontaining less than 0.1 ppm as in 8.3.9. Report9.1 Report the type of tile tested, the volume of acid used,the test cell area, and the lead and cadmium leached in parts permillion for each tile or sample mount tested.9.2 As indicated in Section 1, this procedure covers th
31、eextraction and measurement of lead and cadmium. It is generalin that it does not recommend specific sample types. Forspecial end uses, as for example, process control or interlabo-ratory testing, a specific size and type of sample unit should beused.10. Precision and Bias10.1 In an analysis of vari
32、ance study from eightlaboratories, the standard deviation between laboratories was0.06 mg/L for lead and 0.007 mg/L for cadmium. Thewithin-laboratory precision had a standard deviation of 0.04mg/L for lead and 0.004 mg/L for cadmium. The standarddeviation for interaction between laboratories and sam
33、ples is0.06 mg/L for lead and 0.010 mg/L for cadmium. Reproduc-ibility is defined as the square root of the sum of the threecomponent variances. The reproducibilities were 0.10 mg/L forlead and 0.013 mg/L for cadium.10.2 The bias of this test method is further limited by theability to obtain represe
34、ntative samples of the statistical uni-verse being sampled.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH
35、Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.6To ensure no loss of solution, a silicone rubber, as described, may be used forgrouting. Care should be taken to minimize the amount of grout on the glaze su
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40、 at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 87 (2014)3
