ASTM_D_2085_-_89_2002.pdf

Designation:D 2085 89(Reapproved 2002)Standard Test Method forDetermining Chloride Used in CalculatingPentachlorophenol in Solutions or Wood(Lime IgnitionMethod)1This standard is issued under the fixed designation D 2085;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 procedures cover the chemical analysis by thelime ignition method of treating solutions containing pen-tachlorophenol and of wood treated with pentachlorophenol.The method is suitable for the determination of up to 0.05 g ofpentachlorophenol in treating solutions(Section 8),up to 0.05g of pentachlorophenol in wood volumes up to 0.25 in.3(Section 9),and up to 0.25 g of pentachlorophenol in woodvolumes up to 2.0 in.3(Section 11).1.2 This test method is not applicable to samples containinghalogens other than chlorine unless appropriate correction canbe made.Total halogen(excluding fluorine)is calculated as itspentachlorophenol equivalent of chloride.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.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water23.Summary of Test Method3.1 An excess of silver nitrate is added to a nitric acidsolution containing the chloride.The silver chloride is filteredoff,and the excess of silver is titrated with thiocyanate in thepresence of a ferric salt.Apinkish-brown color is formed whenexcess ferric thiocyanate is produced.4.Significance and Use4.1 This test method covers tests for pentachlorophenolcontent in the treating solutions and the wood specimen.5.Apparatus5.1 Crucibles,iron,nickel,or porcelain.5.2 Ignition Sources:5.2.1 Gas Burner,high-temperature of the Meker type,or5.2.2 Electric Muffle.5.3 Analytical Balance,sensitive to 0.001 g.5.4 Magnetic Stirrer,with stirring bars(optional).5.5 Bchner Funnel.5.6 Suction Flask.5.7 Vacuum Source.5.8 Food Blender,equipped with a detachable lid and bladeassembly that will fit a12-pt fruit jar threaded top(HamiltonBeach Model 215 or equivalent).5.9 Fruit Jar,12-pt,with smooth inside walls and equippedwith a protective cover over the assembly in case of breakageduring blending.(Spraying the inside wall of the jar withsilicone resin will prevent sticking of the lime-boring mixture.)5.10 Miscellaneous Glassware,as required.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.3Other 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 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Specification D 1193.6.3 Ammonium Thiocyanate Solution(Approximately 0.1N)Dissolve 7.6 g of ammonium thiocyanate(NH4CNS)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 Oct.27,1989.Published December 1989.Originallypublished as D 2085 71.Last previous edition D 2085 88.2Annual Book of ASTM Standards,Vol 11.01.3“Reagent Chemicals,American Chemical Society Specifications,”Am.Chemi-cal Soc.,Washington,DC.For suggestions on the testing of reagents not listed bytheAmerican Chemical Society,see“Reagent Chemicals and Standards,”by JosephRosin,D.Van Nostrand Co.,Inc.,New York,NY,and the“United StatesPharmacopeia.”1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.crystals containing 0.005%or less chloride in water.Quanti-tatively transfer to a 1-Lvolumetric flask and add water exactlyto mark.Mix well.Certified,commercially prepared NH4CNSsolutions are suitable.6.4 Calcium HydroxidePowdered calcium hydroxide(Ca(OH)2)containing 0.025%or less chloride.6.5 Ferric Ammonium Sulfate Solution(Volhard Indica-tor)Dissolve 10 g of ferricammonium sulfate(FeNH4-(SO4)212H2O)crystals containing 0.001%or less chloride ina dilute HNO3solution prepared by adding 10 mL of concen-trated HNO3to 100 mL of water.6.6 Lime-Nitrate MixtureThoroughly mix 10 parts ofCa(OH)2with 1 part of the powdered KNO3.6.7 Nitric Acid(sp gr 1.42)Concentrated nitric acid(HNO3),containing 0.00005%or less chloride.6.8 Potassium NitratePotassium nitrate(KNO3)crystalscontaining 0.002%or less chloride.Grind and powder theKNO3using an a