1、Designation: C1606 10Standard Test Method forSampling Protocol for TCLP Testing of ContainerGlassware1This standard is issued under the fixed designation C1606; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. 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 defines the way in which containerglassware should be prepared before performing the ToxicityCharacteristic Lea
3、ching Procedure (TCLP). The method coversthe homogenization of the sample, and the selection of arepresentative portion of the sample to test and get reproduc-ible results.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3
4、This standard does not purport to address all of thesafety 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 to determine theapplicability of regulatory limitations prior to use.2. Referenced Docu
5、ments2.1 ASTM Standards:2E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE177 Practice for Use of the Terms Precision and Bias inASTM Test Methods3. Summary of Test Method3.1 Container glass articles decorated with ceramic glassdecorations are broken t
6、o fit the requirements of the TCLPprotocol by using a disc mill or roll mill apparatus, and then thesamples are homogenized using a riffle box. A representativesample of the glass articles can then be put through the TCLPtest with reproducible results.4. Significance and Use4.1 Sampling of decorated
7、 glass containers for the TCLPcan vary greatly, resulting from the size and shape of the articlerelative to the amount of ceramic decoration on the ware.Breaking the glass can cause some of the pieces to have nodecoration on them, and others to be heavily decorated andmore likely to leach lead and c
8、admium under the TCLP test.This method provides an effective tool to homogenize the glasscontainers so that reproducible results can be attained from theTCLP test.5. Apparatus5.1 Pre-breaking apparatus, consisting of:5.1.1 Two L (or larger) polythene bucket with a tightlysealed lid,5.1.2 One or two
9、clean 35 to 40 mm diameter aluminagrinding balls,5.2 Disc mill or roll mill,5.3 Sieves, as needed,5.4 Riffle box, and5.5 Roller or tumbler apparatus.6. Reagents and Materials6.1 Glassware to be tested, in two sets of 10 units each.7. Hazards7.1 When working with glassware, always be aware andcareful
10、 of the potential of getting cut by the glass. Personalprotective equipment, such as a face shield or goggles, leathergloves, and a protective apron should be worn when workingwith glass.Take precautions when working with the samples andapparatus to avoid the possibilities of getting hurt.8. Samplin
11、g, Test Specimens, and Test Units8.1 Since the amount of lead and cadmium that leaches froma decoration can be affected by the relative size of thedecoration, it is important to start with two sets of 10 unitseach.1This test method is under the jurisdiction ofASTM Committee C21 on CeramicWhitewares
12、and Related Products and is the direct responsibility of SubcommitteeC21.03 on Methods for Whitewares and Environmental Concerns.Current edition approved Nov. 1, 2010. Published December 2010. Originallyapproved in 2004. Last previous edition approved in 2004 as C160604(2009). DOI:10.1520/C1606-10.2
13、For 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C
14、700, West Conshohocken, PA 19428-2959, United States.9. Procedure9.1 To minimize the variation of sampling, this testing shallbe done in duplicate, and therefore, take two sets of 10 units ofthe glassware to be tested.9.2 Pre-break the glass prior to milling, using the followingprocedure:9.2.1 Place
15、 the first set of glassware into the 2 L bucket,along with one or two clean 35 to 40 mm diameter aluminagrinding balls.9.2.2 After tightly sealing the lid, shake the vessel hardenough to smash the glass to create pieces that can be fed intothe roll or disc mill.9.3 Clean both the mill and riffle box
16、, prior to use.9.4 Feed the pre-broken glass into the disc mill or roll millas feedstock.9.4.1 Grind the glass as two separate lots, with the selectedmill apertures set between 2.5 mm and 3.5 mm. Theseaperature settings tend to produce crushed glass with a maxi-mum particle size of 5 mm.9.5 Any over
17、sized material must be removed by sieving orhand picking, and be broken up prior to blending back into theoriginal sample.9.6 Homogenize the sample using a roller or tumblerapparatus.9.7 Immediately pass sample through the riffle box collect-ing two sub-samples of 100g each.9.8 Perform TCLP extracti
18、on according to EPA specifica-tions.10. Precision and Bias10.1 The precision of this test method is based on aninterlaboratory study of C1606-04 Standard Test Method forSampling Protocol for TCLP Testing of Container Glassware,conducted in 2008. Four laboratories participated in this study.Each of t
19、he labs was asked to report two replicate test resultsfor three different materials, however not every lab reportedreplicate data for each material. Every “test result” that wasreported represents an individual determination. Except for theuse of only four laboratories, and inconsistent reporting of
20、replicates, Practice E691 was followed for the design andanalysis of the data; the details are given in RR:C21-1006.310.1.1 Repeatability limit (r)Two test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more than the “r” value for that material; “r”istheinterva
21、l representing the critical difference between two testresults for the same material, obtained by the same operatorusing the same equipment on the same day in the samelaboratory.10.1.1.1 Repeatability limits are listed in Table 1 and Table2.10.1.2 Reproducibility limit (R)Two test results shall beju
22、dged not equivalent if they differ by more than the “R” valuefor that material; “R” is the interval representing the criticaldifference between two test results for the same material,obtained by different operators using different equipment indifferent laboratories.10.1.2.1 Reproducibility limits ar
23、e listed in Table 1 andTable 2.10.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.10.1.4 Any judgment in accordance with statements 10.1.1and S101 would normally have an approximate 95 % probabil-ity of being correct, however the precision
24、statistics obtained inthis ILS must not be treated as exact mathematical quantitieswhich are applicable to all circumstances and uses. The limitednumber of materials tested and laboratories reporting resultsguarantees that there will be times when differences greaterthan predicted by the ILS results
25、 will arise, sometimes withconsiderably greater or smaller frequency than the 95 %probability limit would imply. The repeatability limit and thereproducibility limit should be considered as general guides,and the associated probability of 95 % as only a roughindicator of what can be expected.10.2 Bi
26、asAt the time of the study, there was no acceptedreference material suitable for determining the bias for this testmethod, therefore no statement on bias is being made.10.3 The precision statement was determined through sta-tistical examination of 32 results, from four laboratories, onthree material
27、s.To judge the equivalency of two test results, it is recom-mended to choose the material closest in characteristics to thetest material.11. Keywords11.1 TCLP; ceramic glass enamels; ceramic glassdecorations3Supporting data have been filed at ASTM International Headquarters and maybe obtained by req
28、uesting Research Report RR:C21-1006.TABLE 1 Pb (ppm)Material AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitx srsRrRPochet 0.47 0.08 0.44 0.22 1.23FB 2.17 2.12 2.96 5.95 8.28Green 0.00 0.00 0.00 0.00 0.00AThe average of the laboratories ca
29、lculated averages.C1606 102ASTM 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 validity of any such patent rights, and the riskof infri
30、ngement 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 comments are invited either for revision of this standar
31、d 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 have not received a fair hearing you shouldmake your view
32、s 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 multiple copies) of this standard may be obtained by contactin
33、g 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Cd (ppm)Material AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitx sr sR r RPochet 0.02 0.00 0.04 0.00 0.10FB 0.18 0.22 0.31 0.61 0.88Green 0.00 0.00 0.00 0.00 0.00AThe average of the laboratories calculated averages.C1606 103
