1、Designation: C 927 80 (Reapproved 2004)Standard Test Method forLead and Cadmium Extracted from the Lip and Rim Area ofGlass Tumblers Externally Decorated with Ceramic GlassEnamels1This standard is issued under the fixed designation C 927; the number immediately following the designation indicates th
2、e year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of lead
3、 andcadmium extracted by acetic acid from the lip and rim area ofglassware used for drinking and which is exteriorly decoratedwith ceramic glass enamels. The procedure of extraction maybe expected to accelerate the release of lead and cadmium fromthe decorated area and to serve, therefore, as a seve
4、re test thatis unlikely to be matched under the actual conditions of usageof such glassware. This test method is specific for lead andcadmium.NOTE 1For additional information see Test Method C 738.1.2 The values stated in acceptable metric units are to beregarded as the standard. The values given in
5、 parentheses arefor information only.1.3 This standard may involve hazardous materials, opera-tions, and equipment. This standard does not purport toaddress all of the safety concerns associated with its use. It isthe responsibility of the user of this standard to establishappropriate safety and hea
6、lth practices and determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C 738 Test Method for Lead and Cadmium Extracted fromGlazed Ceramic Surfaces3. Terminology3.1 Definitions:3.1.1 ceramic glass decorationsceramic glass enamelsfused to glassw
7、are at temperatures above 425C (800F) toproduce a decoration.3.1.2 ceramic glass enamels (also ceramic enamels or glassenamels)predominately colored, silicate glass fluxes used todecorate glassware.3.1.3 lip and rim areathat part of a drinking vessel whichextends 20 mm below the rim on the outside o
8、f the specimen.4. Summary of Test Method4.1 Lead and cadmium are extracted from the lip and rimarea of the article under test by leaching with a 4 % acetic acidsolution at 20 to 24C (68 to 75F) for 24 h and are measuredby atomic absorption spectrophotometry using specific hollowcathode or electrodel
9、ess discharge lamps for lead and cadmiumrespectively. Results are reported as micrograms per millilitre(ppm) extracted relative to the internal volume of the glassarticle.5. Significance and Use5.1 The heavy metals, lead and cadmium, are known tocause serious health effects in man if consumed in exc
10、ess. It is,therefore, important to measure the amount that may beextracted from an area of the glass drinking vessel in contactwith the lip. Even though the amount of lead and cadmiumextracted by this test method is in no way representative of theamount of the metals extracted by actual lip contact,
11、 therelative magnitude of metals extracted from one test specimenin relation to another test specimen provides an effective toolfor discrimination.6. Interferences6.1 Since specific hollow cathode lamps or electrodelessdischarge lamps for lead and cadmium are used, there are nointerferences.7. Appar
12、atus7.1 Atomic Absorption Spectrophotometer (AAS), equippedwith a 102-mm (4-in.) single slot or Boling burner head anddigital concentration readout attachment (DCR) if available.This instrument should have a sensitivity of about 0.5 g/mL of1This test method is under the jurisdiction of ASTM Committe
13、e C14 on Glassand Glass Products and is the direct responsibility of Subcommittee C14.10 onGlass Decoration. It was developed jointly by ASTM Committee C-14 and C-21 onCeramic Whitewares and Related Products, the Society of Glass Decorators A-20Subcommittee on Ceramic Enameled Decorated Glass Tumble
14、rs, and an Inter-agency Task Force consisting of FDA, EPA, and CPSC of the U.S. Government.Current edition approved Oct. 1, 2004. Published October 2004. Originallyapproved in 1980. Last previous edition C 927 - 80 (1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontac
15、t ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.lead for 1 % absorption
16、and a sensitivity of about 0.025 g/mLof cadmium for 1 % absorption. Use the operating conditionsas specified in the instrument manufacturers analytical meth-ods manual.7.2 Hollow Cathode or Electrodeless Discharge LeadLamp, set at 283.3 nm.7.3 Hollow Cathode or Electrodeless Discharge CadmiumLamp, s
17、et at 228.8 nm.7.4 Glassware of chemically resistant borosilicate glass foruse in preparing and storing reagents and solutions, and for useas test specimen containers.7.5 Detection limits of lead and cadmium shall be deter-mined and reported for individual instruments. In this testmethod, the detect
18、ion limit shall be defined as twice the meannoise level at 0 g/mL. Representative detection limits wouldbe approximately 0.01 to 0.03 g/mL for lead and 0.0005 to0.0010 g/mL for cadmium.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it
19、is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused provided it is first ascertained that the reagent is ofsufficiently high purity to permit its us
20、e without lessening theaccuracy of the determination. Analyze each new batch ofreagents for lead and cadmium.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled or deionizedwater.8.3 Acetic Acid (4 volume %)Mix 1 volume of glacialacetic acid with 2
21、4 volumes of water.8.4 Cadmium Standard Stock Solution (1000 g/mL ofcadmium)Dissolve 0.9273 g of anhydrous cadmium sulfatein 250 mL of 1 % HCl (8.6) and dilute to 500 mL with 1 %HCl. Commercially available standard cadmium solutions mayalso be used.8.5 Detergent RinseAdd 2 mL of hand dishwashingdete
22、rgent to 1 L of lukewarm tap water.8.6 Hydrochloric Acid (1 weight %)Mix 1 volume ofconcentrated hydrochloric acid (HCl, sp gr 1.19) with 37volumes of water.8.7 Lead Standard Stock Solution (1000 g/mL)Dissolve1.598 g of lead nitrate (Pb(NO3)2) in 4 % acetic acid and diluteto 1 L with 4 % acetic acid
23、. Commercially available standardlead solutions may also be used.9. Sampling9.1 Continuous ProcessSince the amount of metal re-leased from a decoration can be affected by the firing condi-tions, which may not be uniform across the width of the lehr,a minimum of six samples should be taken representi
24、ng bothsides and the center of the lehr.9.2 Load or PileA minimum of six samples should berandomly selected from throughout the load.10. Preparation of Standards10.1 Lead Standard Working SolutionsDilute lead nitratesolution (8.7) with acetic acid (8.3) to obtain working standardshaving final lead c
25、oncentrations of 0, 5, 10, 15, and 20 g/mL.10.2 Cadmium Standard Working SolutionsDilute cad-mium stock solution (8.4) with acetic acid (8.3) to obtainworking standards having final cadmium concentrations of 0.0,0.3, 0.5, 1, 1.5, and 2.0 g/mL.10.3 Fresh working solutions should be prepared daily.11.
26、 Procedure11.1 Preparation of SampleTake six identical units andcleanse each with a detergent rinse. Then rinse with tap waterfollowed by distilled water followed by air drying. Mark eachunit 7 mm below the rim. Record the internal volume of eacharticle in millilitres by filling from a graduated cyl
27、inder toapproximately 6 to 7 mm (14 in.) of overflowing. Mark eacharticle, in a nondecorated area (if possible), 20 mm below therim on the outside. Invert the article in an appropriate labora-tory glassware container whose diameter is a minimum of 1.25times and a maximum of 2.0 times the diameter of
28、 the testspecimen at the rim. Carefully add 4 % acetic acid leachingsolution from a graduated cylinder to the 20-mm mark. Recordthe volume of solution used. Cover the glassware containers, ifpossible, to prevent evaporation and to protect them fromcontamination. Let stand for 24 h at room temperatur
29、e (20 to24C) in the dark. Remove the article after the 24-h leachingperiod and determine the lead and cadmium by atomic absorp-tion. Record the lead and cadmium found in micrograms permillilitre.NOTE 2The possibility of a significant amount of evaporation exists.The analyst should determine whether
30、the acetic acid leaching is notice-ably below the 20-mm mark before removing the article. If it is, sufficientacetic acid solution should be added to restore the leaching solution to the20-mm mark.11.2 Determination of LeadSet the instrument (7.1) formaximum signal at 283.3 nm using the lead hollow
31、cathodelamp (7.2) (Note 3) and air/acetylene (C2H2) flow ratesrecommended by the manufacturer. Stir the sample (leaching)solution and pour off a portion into a clean flask or aspiratefrom the extraction container if suitable. Flush the burner withwater and check zero point between readings. Determin
32、e leadfrom a standard curve of absorbance against g/mL of lead orcalibrate the direct concentration reading (DCR) unit in theconcentration mode with lead working solutions (11.1) andread and record the sample concentration directly. Bracket thesample solution with the next higher and lower workingso
33、lutions. Dilute samples containing more than 20 g/mL oflead with 4 % acetic acid and reanalyze.NOTE 3Electrodeless discharge lamps may be substituted for hollowcathode lamps.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the
34、 testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.C 927 80 (2004)211.3 Determination of Cadmi
35、umProceed as in 11.2 usingthe cadmium hollow cathode lamp (7.3) and cadmium stan-dards (10.2). If the sample (leaching) solution contains morethan 2 g/mL of cadmium, dilute with 4 % acetic acid andreanalyze.12. Calculation12.1 Use the following equations to calculate the totalamount of lead or cadmi
36、um metal released from the lip and rimarea of the article expressed (1) in total micrograms and (2)parts per million of lead or cadmium metal leached relative tothe internal volume of the article.12.1.1 Determine lead or cadmium, A, in micrograms asfollows:A 5 C 3 V1(1)12.1.2 Determine lead or cadmi
37、um, A, in parts per millionas follows:A 5C 3 V1V2(2)where:C = concentration of lead or cadmium in leaching solu-tion, g/mL;V1= volume of leaching solution, mL; andV2= internal volume of article, mL (Note 4).NOTE 4The internal volume of the article expressed in millilitres ofwater closely approximate
38、s its weight in grams. Therefore, in this instancemicrogram per millilitre equals microgram per gram which equals partsper million.13. Report13.1 A suggested report form is given in Fig. 1.14. Precision and Bias14.1 Precision for the analytical method for single ormultiple operator within a single l
39、aboratory is within thesensitivity of the AAS used and as specified is about 0.5 g/mLfor lead and 0.25 g/mL for cadmium.14.2 The accuracy and between-laboratory precision aredependent upon the ability to obtain representative samples forthe statistical universe being sampled.15. Keywords15.1 atomic
40、absorption; cadmium; ceramic glass enamels;glaze; heavy metals; leadC 927 80 (2004)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the
41、 validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your
42、 comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments
43、have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multi
44、ple copies) of this standard may be obtained by contacting ASTM 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).LABORATORY TEST DATALead and Cadmium Released from Lip and Rim Area of Drinking Glassware Decorat
45、ed Externally with Ceramic Glass EnamelsDateManufacturer LaboratoryPatternDetection Limit Lead Reagent Blank LeadCadmium CadmiumInternal Volume, mLSample Volume of Leach-ing Solution, mLConcentration, g/mLLead,Total g ppm Relative toInternal Volume123456AvgCadmium123456AvgFIG. 1 Report FormC 927 80 (2004)4
