Designation:D5517−14
Standard Test Method for
Determining Extractability of Metals from Art Materials1
This standard is issued under thefixed designation D5517;the number immediately following the designation indicates the year of original adoption or,in the ca of revision,the year of last revision.A number in parenthes indicates the year of last reapproval.A superscript epsilon(´)indicates an editorial change since the last revision or reapproval.
1.Scope
1.1This test method covers the extraction of metals from art materials using an extractant that simulates the acid potential of gastric juice.This test method is similar to the extraction method in Specification F963,except that it requires conduct-ing extraction steps at body temperature instead of at room temperature.The extraction procedure specified in this test method is more rigorous than that noted in Specification F963 becau the procedure caus the extraction of a larger quantity of metal.
1.2This test method is adapted from the European Toy Safety Standard,EN71-3:1994but differs from it in that a solvent extraction step is not required for processing waxes or oil-bad products and no specific acceptable metal levels are specified.
1.3The rational for this test method is discusd in Appen-dix X1.
1.4This test method should be ud on the art material as a whole and not an art material ingredient.Testing the art material as whole would be expected to give a more accurate estimate of soluble metal than from an extrapolation from testing ingredients.
1.5The values stated in SI units are to be regarded as standard.No other units of measurement are included in this standard.
1.6This standard does not purport to address all of the safety concerns,if any,associated with its u.It is the responsibility of the ur of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to u.
2.Referenced Documents
2.1ASTM Standards:2
D4236Practice for Labeling Art Materials for Chronic Health Hazards
E180Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn2009)3
E456Terminology Relating to Quality and Statistics
F963Consumer Safety Specification for Toy Safety
头皮痒痒怎么回事
2.2International Standards:4
EN71-3:1994Safety of Toys
ISO3696Water for Laboratory U—Specifications
ISO3856Paints and Varnishes—Determination of “Soluble”Metal Content
Part1:Determination of lead content—Flame atomic ab-sorption spectrometric method and dithiazone spectropho-tometric method
Part2:Determination of antimony content—Flame atomic absorption spectrophotometric method and Rhodamine B spectrophotometric method
Part3:Determination of barium content—Flame atomic emission spectrometric method
信仰歌词Part4:Determination of cadmium content—Flame atomic absorption spectrometric method and polarographic method
Part5:Determination of hexavalent chromium content of the pigment portion of the liquid paint or the paint in powder form—Diphenylcarbazide spectrophotometric method Part6:Determination of total chromium content of the liquid portion of paint—Flame atomic absorption spectrometric method
2.3USEP A Standards:5
USEPA Test Method SW-846
1This test method is under the jurisdiction of ASTM Committee D01on Paint and Related Coatings,Materials,and Applications and is the direct responsibility of Subcommittee D01.57on Artist Paints and Related Materials.
Current edition approved Jan.1,2014.Published February2014.Originally approved in1994.Last previous edition approved in2007as D5517–07.DOI: 10.1520/D5517-14.
2For referenced ASTM standards,visit the ASTM website,www.astm,or contact ASTM Customer Service at rvice@astm.For Annual Book of ASTM Standards volume information,refer to the standard’s Document Summary page on the ASTM website.
3The last approved version of this historical standard is referenced on www.astm.
4Available from European Committee for Standardization(CEN),36rue de Stassart,B-1050,Brusls,be.
5Available from United States Environmental Protection Association(EPA), Ariel Rios Bldg.,1200Pennsylvania Ave.,NW,Washington,DC20460, v.
6010Test Method for antimony,arnic,barium,beryllium, cadmium,chromium,cobalt,copper,lead,mangane, molybdenum,nickel,lenium,silver,thallium, vanadium,and zinc
6020Test Method for aluminum,antimony,arnic,barium, beryllium,cadmium,chromium,cobalt,copper,lead, mangane,nickel,silver,thallium,and zinc
7040Test Method for antimony
7041Test Method for antimony
7060Test Method for arnic
7061Test Method for arnic
7080Test Method for barium
7090Test Method for beryllium
7091Test Method for beryllium
7130Test Method for cadmium
7131Test Method for cadmium
7190Test Method for chromium
7191Test Method for chromium
7200Test Method for cobalt
7201Test Method for cobalt
7210Test Method for copper
7421Test Method for lead
7460Test Method for mangane
7470Test Method for mercury
7471Test Method for mercury
7480Test Method for molybdenum
7481Test Method for molybdenum
7520Test Method for nickel
7550Test Method for osmium
7740Test Method for lenium
7741Test Method for lenium
7760Test Method for silver
7840Test Method for thallium
7841Test Method for thallium
7870Test Method for tin
7910Test Method for vanadium
7911Test Method for vanadium
7950Test Method for zinc
3.Terminology
3.1Definitions:
无理方程3.1.1For formal definitions of statistical terms e Termi-nology E456.
3.2Definitions of Terms Specific to This Standard:
3.2.1ba material,n—material upon which coatings are deposited or formed.
3.2.2bioavailability,n—the extent that a substance can be absorbed in a biologically active form.
3.2.3coating,n—all layers of material covering the ba material.
3.2.4detection limit,n—three times the standard deviation of the blank value.
3.2.5scraping,v—removal of a coating down to the ba material without removing any portion of the ba material;the u of solvents is not permitted.
4.Summary of Test Method
4.1A powdered,liquid,comminuted or ground art material is mixed with a0.07N hydrochloric acid solution and,after adjusting the pH to1.5,is shaken for1h and then allowed to sit for an additional hour.The extraction steps are conducted at3762°C.Solids are parated from the extractant by centrifugation andfiltration through a0.45-µmfilter.The resultant eluate is then analyzed for the metal(s)of interest.
5.Significance and U
5.1This acid extraction method is intended to indicate the solubility of metals from art materials in a weak acid medium. This test method may be uful as one indicator of the amount of metal that is readily available for absorption.It is not meant as a replacement for in vivo tests of absorption of a metal.6 Other relevant information,when available,should be included in the overall toxicological asssment of metal-containing art materials,such as physico-chemical properties,toxicokinetics (absorption,distribution,metabolism and excretion),and mechanisms of toxicity of the metal(s)of interest.
技师论文5.2Maximum levels of metal extraction are en with this test method when results are250ppm or les
s.If results are greater than250ppm,the extractant volume should be in-cread to100mL.7
6.Apparatus
6.1Metal Sieve of aperture0.5mm.
6.2pH meter with an accuracy of60.1pH units.
6.3Membrane Filter with a pore size of0.45µm.
6.4Centrifuge able to centrifuge at a minimum of13600g.
6.5Precision Reciprocal Shaker150oscillations/min with1 in.stroke length or wrist-action shaker capable of controlling the shaking amplitude to462mm and the frequency to96 2Hz.
6.6Constant Temperature Water Bath at3762°C.
7.Reagents
7.1Hydrochloric Acid(0.07N)—Add2.55g concentrated hydrochloric acid(HCl)to water and dilute to1L with water.
7.2Hydrochloric Acid(0.14N)—Add5.10g concentrated hydrochloric acid(HCl)to water and dilute to1L with water.
7.3Hydrochloric Acid(2.0N)—Add72.9g concentrated hydrochloric acid(HCl)to water and dilute to1L with water.
7.4Hydrochloric Acid(6.0N)—Add218.8g concentrated hydrochloric acid(HCl)to water and dilute to1L with water.
7.5Water,of at least Grade3purity in accordance with ISO 3696.
6Supporting data have beenfiled at ASTM International Headquarters and may be obtained by requesting Rearch Report RR:D01-1120.Contact ASTM Customer Service at rvice@astm.
7Supporting data have beenfiled at ASTM International Headquarters and may be obtained by requesting Rearch Report RR:D01-1121.Contact ASTM Customer Service at
rvice@astm.
8.Preparation of Test Portions
8.1A test portion is approximately100mg.
泉州市安全教育平台8.2Art materials that are in the form of a liquid,dust or comminuted solid or are metals,are tested without further preparation.
8.3Scraped coatings of art materials are prepared by com-minuting the sample sufficient to pass through a0.5-mm sieve.
8.4Films,textiles,and paper are prepared by cutting into approximately6by6mm squares.
8.5Solids are comminuted,ground or scraped to prepare a sample sufficient to pass through a0.5mm sieve.
8.6100to200mg of oil-bad mi-solids should be spread on acid washed Whatman40filter paper circles(9cm)prior to extraction.
回车符号怎么去掉9.Procedure
9.1Mix the test portion with50times its mass of an aqueous solution of0.07N hydrochloric acid at3762°C.In ca there is less than a100mg test portion,mix the portion with5.0mL of this solution at the given temperature.Shake for 1min.
9.2Check the acidity of the mixture.If the pH is greater than1.5add drop wi while shaking an aqueous solution of 2N hydrochloric acid until the pH is between1.0and1.5.If a pH meter is ud,appropriate precautions to prevent cross-contamination should be taken.Protect the mixture from light. Shake the mixture efficiently for1h and then allow the mixture to stand for1h at3762°C.
N OTE1—It has been shown that the extraction of soluble cadmium can show a2to5fold increa when extraction is carried out in the light rather than in dark.Using brownflasks or aluminum foil-coveredflasks will eliminate light effects.
9.3If necessary,centrifuge the mixture and parate the solids from the mixture byfiltration through a membranefilter with a pore size of0.45µm.
N OTE2—Somefine pigments may break through a standard0.45-µm filter.In the cas centrifugation of the eluate at13600g for15min will remove remaining suspended pigment particles.
9.4Paper products are prepared byfirst macerating the test portion with25times its mass of water at3762°C so that the resulting mixture is uniform in color and texture.This mixture is than transferred quantitatively to a conicalflask.Add25 times the mass of the test portion of an aqueous solution of 0.14N hydrochloric acid at3762°C and shake for1min. Complete the extraction as in8.2and8.3.
9.5If a test portion contains large quantities of alkaline materials,generally in the form of calcium carbonate,adjust the pH to1.0to1.5with6N hydrochloric acid in order to avoid over dilution.
9.6Determine metal(s)concentration in eluate with the appropriate analytical procedure(e ISO3856or USEPA Test Method SW-846).
10.Calculation
10.1Determine the extractable metal level in a test sample in ppm(mg of metal per kg of test material)as follows: Metal concentration in sample~ppm!
遥远的天国5@metal concentration in eluate~ppm!#
3@eluate volume~mL!#/@sample weight~gm!#(1) 11.Precision and Bias
11.1Precision—The precision estimates are bad on an interlaboratory study8in which one operator in17different laboratories analyzed identically prepared test materials in duplicate using the method specified in this test method. Precision of the extraction was estimated by analys of a comminuted paint sample and the acid extract of this sample. Repeatability and reproducibility standard deviations and95% limits are determined as specified in Practice E180.
11.1.1Repeatability—The within-laboratory standard de-viations and95%repeatability limits for testing three metals are reported in Table1and Table2.
11.1.2Reproducibility—The between-laboratory standard deviations and95%reproducibility limits for testing three metals are reported in Table1and Table2.
11.1.3Bias—No systematic errors were detected between measured and true values on either intralaboratory or between laboratory testing.
12.Keywords
12.1art materials;bioavailability;soluble metals
中国汉字的魅力8Supporting data have beenfiled at ASTM International Headquarters and may be obtained by reque
sting Rearch Report RR:D01-1084.Contact ASTM Customer Service at rvice@astm.
TABLE1Comminuted Paint Sample
Barium Cadmium Chromium Mean value(mg/kg)10122.727.2 Degrees of freedom121413 Repeatability standard deviation 6.00.9 1.66 Repeatability95%limits±17±2.5±4.6 Reproducibility standard deviation21 4.9 3.74 Reproducibility95%limits±48±14±10
TABLE2Acid Extract of Comminuted Paint Sample
Barium Cadmium Chromium Mean value(mg/l) 1.900.4310.513 Degrees of freedom121413 Repeatability standard deviation0.060.010.029 Repeatability95%limits±0.17±0.028±0.081 Reproducibility standard deviation0.360.0510.062 Reproducibility95%limits±1.0±0.13
±0.17
APPENDIX (Nonmandatory Information) X1.RATIONALE
X1.1Practice D4236requires that a toxicologist shall take into account the bioavailability of potentially toxic components of an art material in making a determination whether or not the art material would require labeling for a chronic health hazard. This test method may provide an estimate of the bioavailability after ingestion of lected metals in art materials.
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