ASTM_D_453_-_94_2000e1.pdf

Designation:D 453 94(Reapproved 2000)e1Standard Test Method forTar Acids in Creosote-Coal Tar Solutions1This standard is issued under the fixed designation D 453;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.This standard has been approved for use by agencies of the Department of Defense.e1NOTEA keyword was added editorially in March 2000.1.Scope1.1 This test method covers the determination of tar acids increosote and creosote-coal tar solution.1.1.1 Test Method D 38 covers the sampling of woodpreservatives prior to testing.1.2 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.2.Referenced Documents2.1 ASTM Standards:D 38 Test Methods for Sampling Wood Preservatives Priorto Testing2D 95 Test Method for Water in Petroleum Products andBituminous Materials by Distillation3D 246 Test Method for Distillation of Creosote andCreosote-Coal Tar Solutions2D 836 Specification for Industrial Grade Benzene4D 843 Specification for Nitration Grade Xylene4E 1 Specification for ASTM Thermometers52.2British Wood Preserving Association Standard:British Standard 144 on Wood Preservation63.Summary of Test Method3.1 Acoustic solution is separated and acidified with H2SO4to liberate tar acids that are measured in a graduated funnel.4.Significance and Use4.1 This test method covers the determination of tar acidcontent of creosote coal tar solutions so that comparison can bemade with existing international standards,for example,Brit-ish Standard 144.5.Apparatus5.1 Creosote Distillation Equipment,as described in TestMethod D 246.5.2 Separatory FunnelsTwo Squibb-type separatory fun-nels with stoppers,250-mL capacity.5.3 Type II Separatory FunnelThe Type II glass separa-tory funnel shall have a total capacity of not less than 260 mLand not more than 650 mL,and shall conform to the require-ments shown in Fig.1 except that the bulb at the top may bereplaced by a 500-mL Squibb-type bulb.The capacity of thelower bulb from the stopcock to the first graduation mark shallbe 65.0 mL,and above this mark the stem shall be graduatedaccurately to a total capacity of 100.0 mL in 0.2-mL incre-ments.The graduation marks shall be numbered for each 2 mL.5.4 ThermometerAn ASTM Low Softening Point Ther-mometer having a range from 2 to 80C conforming to therequirements for Thermometer 15C as described in Specifica-tion E 1 or other thermometer of suitable range and precision.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Sodium Hydroxide Solution(20%)Mix 200 g of 50%sodium hydroxide(NaOH)solution with 300 g of water.NOTE1Carbonate-free(clear)50%NaOH solution may be pur-chased and is convenient and safe to use.1This test method is under the jurisdiction of ASTM Committee D07 on Woodand is the direct responsibility of Subcommittee D07.06 on Treatments for WoodProducts.Current edition approved April 15,1994.Published June 1994.Originallypublished as D 453 37.Last previous edition D 453 86.2Annual Book of ASTM Standards,Vol 04.10.3Annual Book of ASTM Standards,Vol 05.01.4Annual Book of ASTM Standards,Vol 06.04.5Annual Book of ASTM Standards,Vol 14.03.6Available from Premier House,150 South Hampton Row,London,England,WUC 1BSAL.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.6.3 Sulfuric Acid Solution(40%)Mix 100 g of concen-trated sulfuric acid(H2SO4,sp gr 1.84)carefully with stirringinto 150 g of water.6.4 Benzene(C6H6)Industrial grade,meeting the require-ments of Specification D 836.6.5 Xylene(C6H4(CH3)2)Nitration grade,meeting therequirements of Specification D 843.7.Preparation of Sample7.1 Warm the sample,if necessary,to dissolve crystallinematerial before taking portion for analysis.Determine watercontent of the sample by Test Method D 95.8.Procedure8.1 Distill 100 g of the sample,weighed to the nearest 0.1 g,to 355C by the procedure described in Test Method D 246,and collect the distillate in a Squibb-type separatory funnel.Add 50 mL of C6H6to the freshly distilled fraction and extractthe resulting solution with three successive 30-mL portions of20%NaOH solution.After each portion of caustic solution isplaced in