ASTM_D_6260_-_98.pdf

Designation:D 6260 98Standard Test Method forGravimetric Determination of Carbon Black in NylonMaterials(PA)1This standard is issued under the fixed designation D 6260;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.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 is applicable to the determination ofcarbon black in a specific class of nylon materials,weatherstable,listed in the property tables of Classification SystemD 4066.1.2 The values stated in SI units are to be regarded as thestandard.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 determine the applica-bility of regulatory limitations prior to use.See Note 2 andNote 3 for specific hazard statements.NOTE1There is no similar or equivalent ISO standard.2.Referenced Documents2.1 ASTM Standards:D 833 Terminology Relating to Plastics2D 1898 Practice for Sampling of Plastics2D 4066 Classification System for Nylon Materials33.Terminology3.1 DefinitionsTerms applicable to this test method aredefined in Terminology D 833.4.Significance and Use4.1 Carbon black is an additive in a specific class of nylonmaterials,weather stable,listed in the property tables ofClassification System D 4066.4.2 This test method determines the presence and level ofcarbon black to ensure the suitability of the nylon material inweatherable applications.5.Apparatus5.1 Normal Laboratory Apparatus.5.2 Filtering Apparatus,capable of containing fine particlesof carbon black.Systems that have been used successfullyinclude the following:5.2.1 Millipore Filter Holder,Glass Microanalysis SystemB,Catalog Number XX100253,with Nucleapore Polycarbon-ate Filters,Type PC,0.2 m,25 mm diameter.5.2.2 Good Crucible with Glass Microfiber Filters,What-man Catalog Number 1825024,2.4 cm GF/F.5.3 Drying Oven,capable of minimum 70C temperature.6.Reagents6.1 Acids for the hydrolysis step should be chosen by theuser for the specific nylon under test.6.1.1 For Nylon 6 and 661+1 hydrochloric acid.Preparein a hood by slowly mixing one part reagent grade HCl into onepart deionized water.6.1.2 For Nylon 6121+1 nitric acid.Prepare as in 6.1.1.NOTE2Use caution.Never mix water into an acid.Continually mix,slowly,in an open flask,when adding acid to water.NOTE3Hydrochloric and nitric acids are corrosive liquids.Wearrubber gloves,rubber apron,and chemical goggles when handling theacids and their solutions.7.Test Specimens7.1 Sample the material in accordance with Practice D 18987.2 Specimens should contain less than 0.3%moisture toavoid weighing errors.8.Procedure8.1 Perform the hydrolysis step in a hood.8.2 Into a clean,dry,250 ml Erlenmeyer flask,transfer asample(weighed to the nearest 0.0001 g)that will yield 20 to100 mg of carbon black.Record the sample weight.8.3 Add,by graduated cylinder,100 mL of the appropriateacid solution and attach a water-cooled condenser.8.4 Apply heat until the sample solution just boils.Continueslight boiling for 2 to 3 h.1This test method is under the jurisdiction of Committee D-20 on Plastics and isthe direct responsibility of Subcommittee D20.15 on Nylon Materials.Current edition approved May 10,1998.Published April 1999.2Annual Book of ASTM Standards,Vol 08.01.3Annual Book of ASTM Standards,Vol 08.02.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.8.5 Remove the flask from the condenser without disturbingany material that may have collected in the condenser.8.6 Rinse the material from the condenser with methanoland discard.8.7 Prior to the next step,heat to a boil 200 to 400 mLof theacid solution;this will be used to rinse the sample followingfiltration.8.8 Dry the filter(see 5.2)to a constant weight,record to thenearest 0.0001 g,and place in its holder.Record the weight.Wet the filter with a few milliliters of the acid solution.8.9 Transfer the filter and holder to a vacuum flask.8.10 Carefully filter the hydrolyzed sample solution,underslight vacuum.Immediately after the sample solution hascompleted filtering,begin rinsing with the heated acid solution(must be kept hot during filtration,to avoid erroneous highresults).8.11 At the completion of the filtration,and rinses if needed,transfer the filter to a dried,tared(record weight to nearest0.0001 g)petri dish.8.12 Dry the dish and filter in a vacuum oven for 1 h at70C.Cool in a desiccator for 15 min and record the weight tothe nearest 0.0001 g.NOTE4If there is no presence of mineral or glass(fiber)fillerssuspected conclude the test here and calculate carbon black(see 9.1).8.13 Place the dish and filter in an oxygen plasma low-temperature asher until all organic matter has been destroyed(5t