1、Designation: D5517 14Standard Test Method forDetermining Extractability of Metals from Art Materials1This standard is issued under the fixed designation D5517; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. 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 extraction of metals from artmaterials using an extractant that simulates the acid potential ofgastri
3、c juice. This test method is similar to the extractionmethod in Specification F963, 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 F963beca
4、use 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 leve
5、ls 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 an ex
6、trapolation 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 the use
7、r 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:2D4236 Practice for Labeling Art Materials for ChronicHealth HazardsE180 Practice for Determining the Precision o
8、f ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)3E456 Terminology Relating to Quality and StatisticsF963 Consumer Safety Specification for Toy Safety2.2 International Standards:4EN 71-3:1994 Safety of ToysISO 3696 Water for Laboratory UseSpecificationsIS
9、O 3856 Paints 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 Bspect
10、rophotometric 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 of thepigment portion of the liquid pain
11、t or the paint in powderformDiphenylcarbazide spectrophotometric methodPart 6: Determination of total chromium content of the liquidportion of paintFlame atomic absorption spectrometricmethod2.3 USEPA Standards:5USEPA Test Method SW-8461This test method is under the jurisdiction of ASTM Committee D0
12、1 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.57 on Artist Paints and Related Materials.Current edition approved Jan. 1, 2014. Published February 2014. Originallyapproved in 1994. Last previous edition approved in 2007 as D5517 07. DO
13、I:10.1520/D5517-14.2For 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 approved version of this histori
14、cal standard is referenced onwww.astm.org.4Available from European Committee for Standardization (CEN), 36 rue deStassart, B-1050, Brussels, Belgium, http:/www.cenorm.be.5Available from United States Environmental Protection Association (EPA),Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington,
15、 DC 20460, http:/www.epa.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16010 Test Method for antimony, arsenic, barium, beryllium,cadmium, chromium, cobalt, copper, lead, manganese,molybdenum, nickel, selenium, silver, thallium,v
16、anadium, 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 Method for antimony7060 Test Method for arsenic7061 Test Method for arsenic7080 Test Method
17、 for barium7090 Test Method for beryllium7091 Test Method for beryllium7130 Test Method for cadmium7131 Test Method for cadmium7190 Test Method for chromium7191 Test Method for chromium7200 Test Method for cobalt7201 Test Method for cobalt7210 Test Method for copper7421 Test Method for lead7460 Test
18、 Method for manganese7470 Test Method for mercury7471 Test Method for mercury7480 Test Method 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 t
19、hallium7841 Test Method for thallium7870 Test Method for tin7910 Test Method for vanadium7911 Test Method for vanadium7950 Test Method for zinc3. Terminology3.1 Definitions:3.1.1 For formal definitions of statistical terms see Termi-nology E456.3.2 Definitions of Terms Specific to This Standard:3.2.
20、1 base material, nmaterial upon which coatings aredeposited or formed.3.2.2 bioavailability, 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 bla
21、nk value.3.2.5 scraping, vremoval of a coating down to the basematerial without removing 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, afte
22、radjusting the pH to 1.5, is shaken for 1 h and then allowed tosit for an additional hour. 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 intere
23、st.5. Significance and Use5.1 This acid extraction method is intended to indicate thesolubility 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 vi
24、vo tests of absorption of a metal.6Other relevant information, when available, should be includedin the overall toxicological assessment of metal-containing artmaterials, such as physico-chemical properties, toxicokinetics(absorption, distribution, metabolism and excretion), andmechanisms of toxicit
25、y of the metal(s) of interest.5.2 Maximum levels of metal extraction are seen with 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.76. Apparatus6.1 Metal Sieve of aperture 0.5 mm.6.2 pH meter with an accuracy
26、of 60.1 pH 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
27、9 62 Hz.6.6 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
28、Hydrochloric 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 with ISO3696.6Supportin
29、g data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1120. ContactASTM CustomerService at serviceastm.org.7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1121. Con
30、tactASTM CustomerService at serviceastm.org.D5517 1428. Preparation of Test 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 pr
31、epared by com-minuting the sample sufficient to pass through a 0.5-mm sieve.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.8.6 100 to 200 mg of oil-ba
32、sed semi-solids should be spreadon acid washed Whatman 40 filter paper circles (9 cm) prior toextraction.9. Procedure9.1 Mix the test portion with 50 times its mass of anaqueous solution of 0.07 N hydrochloric acid at 37 6 2C. Incase there is less than a 100 mg test portion, mix the portionwith 5.0
33、mL of this solution at the given temperature. Shake for1 min.9.2 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. Ifa pH meter is used, appropriate precautions to prevent cross-
34、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 when extraction is carried out in the light ratherthan in dark
35、. 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 fine pigments may break through a standard 0.45-mfilter. In t
36、hese 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 theresulting mixture is uniform in color and texture. This mixtureis
37、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 contains large quantities of alkalinematerials, generally in t
38、he 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-846).10. Calculation10.1 Determine the extractable metal leve
39、l in a test samplein ppm (mg of metal per kg of test material) as follows:Metal concentration in sample ppm!5 metal concentration in eluate ppm!#3 eluate volume mL!#/sample weight gm!# (1)11. Precision and Bias11.1 PrecisionThe precision estimates are based on aninterlaboratory study8in which one op
40、erator 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 extract of this sample.Repeatability and reproducibility standard
41、deviations and 95 %limits are determined as specified in Practice E180.11.1.1 RepeatabilityThe within-laboratory standard de-viations and 95 % repeatability limits for testing three metalsare reported in Table 1 and Table 2.11.1.2 ReproducibilityThe between-laboratory standarddeviations and 95 % rep
42、roducibility 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 materials; bioavailability; soluble metals8Supporting data have be
43、en filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1084. ContactASTM CustomerService at serviceastm.org.TABLE 1 Comminuted Paint SampleBarium Cadmium ChromiumMean value (mg/kg) 101 22.7 27.2Degrees of freedom 12 14 13Repeatability standard deviation 6
44、.0 0.9 1.66Repeatability 95 % limits 17 2.5 4.6Reproducibility standard deviation 21 4.9 3.74Reproducibility 95 % limits 48 14 10TABLE 2 Acid Extract of Comminuted Paint SampleBarium Cadmium ChromiumMean value (mg/l) 1.90 0.431 0.513Degrees of freedom 12 14 13Repeatability standard deviation 0.06 0.
45、01 0.029Repeatability 95 % limits 0.17 0.028 0.081Reproducibility standard deviation 0.36 0.051 0.062Reproducibility 95 % limits 1.0 0.13 0.17D5517 143APPENDIX(Nonmandatory Information)X1. RATIONALEX1.1 Practice D4236 requires that a toxicologist shall takeinto account the bioavailability of potenti
46、ally toxic componentsof an art material in making a determination whether or not theart material would require labeling for a chronic health hazard.This test method may provide an estimate of the bioavailabilityafter ingestion of selected metals in art materials.ASTM International takes no position
47、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 infringement of such rights, are entirely their own responsibility.Th
48、is 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 standard or for additional standardsand should be addressed to ASTM Int
49、ernational 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 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 con
