1、Designation: C1606 10 (Reapproved 2014)Standard 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
2、year of 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 defines the way in which containerglassware should be prepared before performing the Toxicity
3、Characteristic Leaching 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
4、 thisstandard.1.3 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.
5、2. Referenced Documents2.1 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 glassdecora
6、tions are broken to 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 Sam
7、pling of decorated 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 t
8、o leach lead and cadmium 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
9、,5.1.2 One or two 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 b
10、e aware andcareful 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 getti
11、ng hurt.8. Sampling, 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
12、CeramicWhitewares and Related Productsand is the direct responsibility of SubcommitteeC21.03 on Methods for Whitewares and Environmental Concerns.Current edition approved Dec. 1, 2014. Published December 2014. Originallyapproved in 2004. Last previous edition approved in 2010 as C1606 10. DOI:10.152
13、0/C1606-10R14.2For 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.Copyright ASTM International, 100 Barr Harbor D
14、rive, PO Box C700, West Conshohocken, PA 19428-2959. United States19. 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 followingprocedu
15、re:9.2.1 Place 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
16、and riffle box, 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 m
17、m.9.5 Any oversized 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
18、 TCLP extraction 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 s
19、tudy.Each of the 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 inconsisten
20、t reporting ofreplicates, 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; “
21、r”istheinterval 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 resu
22、lts shall bejudged 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 Reproducibi
23、lity limits are 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 S1012 would normally have an approximate 95 % prob-ability of being correct, however
24、 the precision statistics ob-tained in this ILS must not be treated as exact mathematicalquantities which are applicable to all circumstances and uses.The limited number of materials tested and laboratories report-ing results guarantees that there will be times when differencesgreater than predicted
25、 by the ILS results will arise, sometimeswith considerably 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
26、be expected.10.2 BiasAt 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 laboratorie
27、s, onthree materials.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 ma
28、ybe obtained by requesting Research Report RR:C21-1006.TABLE1Pb(ppm)Material AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitxsrsRrRPochet 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
29、laboratories calculated averages.C1606 10 (2014)2ASTM 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
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34、 01923, Tel: (978) 646-2600; http:/ AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitxsr 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 10 (2014)3
