1、Designation: D 5517 07Standard Test Method forDetermining Extractability of Metals from Art Materials1This standard is issued under the fixed designation D 5517; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
2、sion. 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 extraction of metals from artmaterials using an extractant that simulates the acid potential ofgas
3、tric juice. This test method is similar to the extractionmethod in Specification F 963, except that it requires conduct-ing extraction steps at body temperature instead of at roomtemperature. The extraction procedure specified in this testmethod is more rigorous than that noted in Specification F 96
4、3because the procedure causes the extraction of a larger quantityof metal.1.2 This test method is adapted from the European ToySafety Standard, EN 71-3:1994 but differs from it in that asolvent extraction step is not required for processing waxes oroil-based products and no specific acceptable metal
5、 levels arespecified.1.3 The rational for this test method is discussed in Appen-dix X1.1.4 This test method should be used on the art material as awhole and not an art material ingredient. Testing the artmaterial as whole would be expected to give a more accurateestimate of soluble metal than from
6、an extrapolation fromtesting ingredients.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of th
7、e 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:2D 4236 Practice for Labeling Art Materials for ChronicHealth HazardsE 180 Practice for Determining the Prec
8、ision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 456 Terminology Relating to Quality and StatisticsF 963 Consumer Safety Specification for Toy Safety2.2 International Standards:3EN 71-3:1994 Safety of ToysISO 3696 Water for Laboratory UseSpecificationsISO 3856 Pa
9、ints and VarnishesDetermination of“Soluble” Metal ContentPart 1: Determination of lead contentFlame atomic ab-sorption spectrometric method and dithiazone spectropho-tometric methodPart 2: Determination of antimony contentFlame atomicabsorption spectrophotometric method and Rhodamine Bspectrophotome
10、tric methodPart 3: Determination of barium contentFlame atomicemission spectrometric methodPart 4: Determination of cadmium contentFlame atomicabsorption spectrometric method and polarographicmethodPart 5: Determination of hexavalent chromium content ofthe pigment portion of the liquid paint or the
11、paint inpowder formDiphenylcarbazide spectrophotometricmethodPart 6: Determination of total chromium content of theliquid portion of paintFlame atomic absorption spectro-metric method2.3 USEPA Standards:4USEPA Test Method SW-8466010 Test Method for antimony, arsenic, barium, beryllium,cadmium, chrom
12、ium, cobalt, copper, lead, manganese,molybdenum, nickel, selenium, silver, thallium, vana-dium, and zinc6020 Test Method for aluminum, antimony, arsenic, barium,beryllium, cadmium, chromium, cobalt, copper, lead,manganese, nickel, silver, thallium, and zinc7040 Test Method for antimony7041 Test Meth
13、od for antimony1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.57 on Artist Paints and Related Materials.Current edition approved June 1, 2007. Published July 2007. Origina
14、lly approvedin 1994. Last previous edition approved in 2003 as D 5517 03.2For 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 A
15、STM website.3Available from European Committee for Standardization (CEN), 36 rue deStassart, B-1050, Brussels, Belgium, http:/www.cenorm.be.4Available from United States Environmental Protection Association (EPA),Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http:/www.epa.gov.1
16、Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7060 Test Method for arsenic7061 Test Method for arsenic7080 Test Method for barium7090 Test Method for beryllium7091 Test Method for beryllium7130 Test Method for cadmium7131 Test Metho
17、d for cadmium7190 Test Method for chromium7191 Test Method for chromium7200 Test Method for cobalt7201 Test Method for cobalt7210 Test Method for copper7420 Test Method for lead7421 Test Method for lead7460 Test Method for manganese7470 Test Method for mercury7471 Test Method for mercury7480 Test Me
18、thod for molybdenum7481 Test Method for molybdenum7520 Test Method for nickel7550 Test Method for osmium7740 Test Method for selenium7741 Test Method for selenium7760 Test Method for silver7840 Test Method for thallium7841 Test Method for thallium7870 Test Method for tin7910 Test Method for vanadium
19、7911 Test Method for vanadium7950 Test Method for zinc3. Terminology3.1 Definitions:3.1.1 For formal definitions of statistical terms see Termi-nology E 456.3.2 Definitions of Terms Specific to This Standard:3.2.1 base material, nmaterial upon which coatings aredeposited or formed.3.2.2 bioavailabil
20、ity, nthe extent that a substance can beabsorbed in a biologically active form.3.2.3 coating, nall layers of material covering the basematerial.3.2.4 detection limit, nthree times the standard deviationof the blank value.3.2.5 scraping, vremoval of a coating down to the basematerial without removing
21、 any portion of the base material; theuse of solvents is not permitted.4. Summary of Test Method4.1 A powdered, liquid, comminuted or ground art materialis mixed with a 0.07 N hydrochloric acid solution and, afteradjusting the pH to 1.5, is shaken for 1 h and then allowed tosit for an additional hou
22、r. These extraction steps are conductedat 37 6 2C. Solids are separated from the extractant bycentrifugation and filtration through a 0.45-m filter. Theresultant eluate is then analyzed for the metal(s) of interest.5. Significance and Use5.1 This acid extraction method is intended to indicate thesol
23、ubility of metals from art materials in a weak acid medium.This test method may be useful as one indicator of the amountof metal that is readily available for absorption. It is not meantas a replacement for in vivo tests of absorption of a metal.55.2 Maximum levels of metal extraction are seen with
24、thistest method when results are 250 ppm or less. If results aregreater than 250 ppm, the extractant volume should be in-creased to 100 mL or greater to keep metal levels in the eluateat a level of 5 ppm or less.66. Apparatus6.1 Metal Sieve of aperture 0.5 mm.6.2 pH meter with an accuracy of 60.1 pH
25、 units.6.3 Membrane Filter with a pore size of 0.45 m.6.4 Centrifuge able to centrifuge at a minimum of 13 600 g.6.5 Precision Reciprocal Shaker 150 oscillations/min with 1in. stroke length or wrist-action shaker capable of controllingthe shaking amplitude to 4 6 2 mm and the frequency to 9 62 Hz.6.
26、6 Constant Temperature Water Bath at 37 6 2C.7. Reagents7.1 Hydrochloric Acid (0.07 N)Add 2.55 g concentratedhydrochloric acid (HCl) to water and dilute to 1 L with water.7.2 Hydrochloric Acid (0.14 N)Add 5.10 g concentratedhydrochloric acid (HCl) to water and dilute to 1 L with water.7.3 Hydrochlor
27、ic Acid (2.0 N)Add 72.9 g concentratedhydrochloric acid (HCl) to water and dilute to 1 L with water.7.4 Hydrochloric Acid (6.0 N)Add 218.8 g concentratedhydrochloric acid (HCl) to water and dilute to 1 L with water.7.5 Water, of at least Grade 3 purity in accordance withISO 3696.8. Preparation of Te
28、st Portions8.1 A test portion is approximately 100 mg.8.2 Art materials that are in the form of a liquid, dust orcomminuted solid or are metals, are tested without furtherpreparation.8.3 Scraped coatings of art materials are prepared by com-minuting the sample sufficient to pass through a 0.5-mm sie
29、ve.8.4 Films, textiles, and paper are prepared by cutting intoapproximately 6 by 6 mm squares.8.5 Solids are comminuted, ground or scraped to prepare asample sufficient to pass through a 0.5 mm sieve.9. Procedure9.1 Mix the test portion with 50 times its mass of anaqueous solution of 0.07 N hydrochl
30、oric acid at 37 6 2C. Incase there is less than a 100 mg test portion, mix the portionwith 5.0 mL of this solution at the given temperature. Shake for1 min.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1120.6Supporting dat
31、a have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1121.D55170729.2 Check the acidity of the mixture. If the pH is greaterthan 1.5 add drop wise while shaking an aqueous solution of2 N hydrochloric acid until the pH is between 1.0 and 1.5. If
32、 apH meter is used, appropriate precautions to prevent cross-contamination should be taken. Protect the mixture from light.Shake the mixture efficiently for 1 h and then allow the mixtureto stand for1hat376 2C.NOTE 1It has been shown that the extraction of soluble cadmium canshowa2to5fold increase w
33、hen extraction is carried out in the light ratherthan in dark. Using brown flasks or aluminum foil-covered flasks willeliminate light effects.9.3 If necessary, centrifuge the mixture and separate thesolids from the mixture by filtration through a membrane filterwith a pore size of 0.45 m.NOTE 2Some
34、fine pigments may break through a standard 0.45-mfilter. In these cases centrifugation of the eluate at 13 600 g for 15 min willremove remaining suspended pigment particles.9.4 Paper products are prepared by first macerating the testportion with 25 times its mass of water at 37 6 2C so that theresul
35、ting mixture is uniform in color and texture. This mixtureis than transferred quantitatively to a conical flask. Add 25times the mass of the test portion of an aqueous solution of0.14 N hydrochloric acid at 37 6 2C and shake for 1 min.Complete the extraction as in 8.2 and 8.3.9.5 If a test portion c
36、ontains large quantities of alkalinematerials, generally in the form of calcium carbonate, adjustthe pH to 1.0 to 1.5 with 6 N hydrochloric acid in order to avoidover dilution.9.6 Determine metal(s) concentration in eluate with theappropriate analytical procedure (see ISO 3856 or USEPATestMethod SW-
37、846).10. Calculation10.1 Determine the extractable metal level in a test samplein ppm (mg of metal per kg of test material) as follows:Metal concentration in sample ppm!5metal concentration in eluate ppm!#3 eluate volume mL!#/sample weight gm!#. (1)11. Precision and Bias11.1 PrecisionThe precision e
38、stimates are based on aninterlaboratory study7in which one operator in 17 differentlaboratories analyzed identically prepared test materials induplicate using the method specified in this test method.Precision of the extraction was estimated by analyses of acomminuted paint sample and the acid extra
39、ct of this sample.Repeatability and reproducibility standard deviations and 95 %limits are determined as specified in Practice E 180.11.1.1 RepeatabilityThe within-laboratory standard de-viations and 95 % repeatability limits for testing three metalsare reported in Table 1 and Table 2.11.1.2 Reprodu
40、cibilityThe between-laboratory standarddeviations and 95 % reproducibility limits for testing threemetals are reported in Table 1 and Table 2.11.1.3 BiasNo systematic errors were detected betweenmeasured and true values on either intralaboratory or betweenlaboratory testing.12. Keywords12.1 art mate
41、rials; bioavailability; soluble metalsAPPENDIX(Nonmandatory Information)X1. RATIONALEX1.1 Practice D 4236 requires that a toxicologist shall takeinto account the bioavailability of potentially toxic componentsof an art material in making a determination whether or not theart material would require l
42、abeling for a chronic health hazard.This test method may provide an estimate of the bioavailabilityafter ingestion of selected metals in art materials.7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1084.TABLE 1 Comminuted P
43、aint SampleBarium Cadmium ChromiumMean value (mg/kg) 101 22.7 27.2Degrees of freedom 12 14 13Repeatability standard deviation 6.0 0.9 1.66Repeatability 95 % limits 617 62.5 64.6Reproducibility standard deviation 21 4.9 3.74Reproducibility 95 % limits 648 614 610TABLE 2 Acid Extract of Comminuted Pai
44、nt SampleBarium Cadmium ChromiumMean value (mg/l) 1.90 0.431 0.513Degrees of freedom 12 14 13Repeatability standard deviation 0.06 0.01 0.029Repeatability 95 % limits 60.17 60.028 60.081Reproducibility standard deviation 0.36 0.051 0.062Reproducibility 95 % limits 61.0 60.13 60.17D5517073ASTM Intern
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47、d 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 views known to the ASTM Committee on Stand
48、ards, 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 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).D5517074
