ASTM_D_1274_-_95_2000.pdf

Designation:D 1274 95(Reapproved 2000)Standard Test Methods forChemical Analysis of Pentachlorophenol1This standard is issued under the fixed designation D 1274;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 These test methods cover the determination of thechemical analysis of pentachlorophenol for use in the preser-vative treatment of wood.1.1.1 Test Method D 38 covers the sampling of woodpreservatives prior to testing.1.2 The analytical procedures appear in the following order:SectionsTotal Acidity6 and 7Alkali-Insoluble Material8 and 9Freezing Point101.3 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.2.Referenced Documents2.1 ASTM Standards:D 38 Test Methods for Sampling Wood Preservatives Priorto Testing2D 1193 Specification for Reagent Water3D 1272 Specification for Pentachlorophenol22.2Other Standard:AWPA A5 Standard Methods for Analysis of Oil-BornePreservatives43.Summary of Test Methods3.1 PentachlorophenolA measured sample is dissolved inmethanol.The phenol is titrated with a standard solution ofSodium Hydroxide.3.2 Sodium Hydroxide Insoluble Matter A weighedsample is digested in 0.1 N NaOH and filtered.The residue isdried and weighed.3.3 Freezing PointA sample is heated in an enameled cupor nickel tube to 10C above the expected melting point,thengradually cooled,and the melting point measured by a stan-dardized thermometer.4.Significance and Use4.1 Pentachlorophenol for use in the preservative treatmentof wood must conform with Specification D 1272.5.Reagents5.1 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.5Other 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.5.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Specification D 1193.TOTAL ACIDITY6.Reagents6.1 Sodium Hydroxide,Standard Solution(0.1 N)Dissolve 4.0 g of sodium hydroxide(NaOH)in 1000 mL ofwater.6.1.1 Standardization of Sodium Hydroxide SolutionTransfer four 0.1 N potassium acid phthalate replicates(from6.2),each of 25.00-mL volume,into 125-mL Erlenmeyerflasks.Add 3 to 5 drops of phenolphthalein indicator solutionto each replicate.Titrate to a permanent faint pink end pointwith 0.1 N NaOH solution(from 6.1).Read the buret to thenearest estimated 0.01 mL.Record the volume of NaOHsolution used for each replicate.1These test methods are under the jurisdiction of ASTM Committee D-7 onWood and are the direct responsibility of Subcommittee D07.06 on Treatments forWood Products.Current edition approved July 15,1995.Published September 1995.Originallypublished as D 1274 53.Last previous edition D 1274 94.These test methods are identical in substance with appropriate sections of theAmerican Wood-Preservers Association Standard Methods for Analysis of Oil-Borne Preservatives(A5-93).Acknowledgment is made to the American Wood-Preservers Association for its development of the subject matter covered in thisstandard.2Annual Book of ASTM Standards,Vol 04.10.3Annual Book of ASTM Standards,Vol 11.01.4Available from American Wood Preservers Association,P.O.Box 286,Woodstock,MD 21163-0286.5Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmaceutical Convention,Inc.(USPC),Rockville,MD.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.6.2 Potassium Acid Phthalate,Standard Solution(0.1 N)Weigh from 18 to 22 g of oven-dry primary standard gradepotassium acid phthalate to the nearest 1 mg.Quantitativelytransfer to a 1-L volumetric flask.Add water exactly to themark.Mix well.6.3 Meta-Cresol Purple Indicator SolutionTransfer 0.1 gm-cresol purple to a small mortar.Add 2.5 mL of 0.1 N NaOHsolution and complete solution with the aid of a pestle.Add100 mL of water.6.4 Phenolphthalein Indicator Solution(5 g/L)Dissolve0.5 g of phenolphthalein in 50 mL of ethanol plus 50 mL ofwater.6.5 Methanol.7.Procedure7.1 Sample PreparationWeigh from 4 to 6 g of oven