ASTM_D_2988_-_96_2015.pdf

Designation:D298896(Reapproved 2015)Standard Test Methods forWater-Soluble Halide Ion in Halogenated Organic Solventsand Their Admixtures1This standard is issued under the fixed designation D2988;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()indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope1.1 Test Methods 1,2,and 3These test methods cover thedetermination of water-extractable halide ion in halogenatedorganic solvents and their admixtures.Fluoride ion is notmeasured due to the solubility of silver fluoride.1.2 Test Method 4This test method covers the determina-tion of chloride ion in halogenated organic solvents and theiradmixtures.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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.Specific precau-tionary statements are given in Section 6.2.Summary of Test Method2.1 Summary of Test Methods 1,2,3Halide ion present inhalogenated organic solvents is extracted with water andprecipitated as the silver halide salt with silver nitrate.Quantityof the halide present is determined by comparing the turbidityof the sample to known standards.The distilled water,as wellas all glassware used,must be halide-free.2.2 Summary of Test Method 4This test method is basedon the determination of ionizable chloride by titration withmercuric acetate solution using s-diphenylcarbazone as theindicator.3.Significance and Use3.1 These test methods are used to establish manufacturingand purchasing specifications.These test methods will providea means of determining the condition of the solvent in use.Ahigh water soluble chloride level may indicate the start ofsolvent decomposition.4.Apparatus4.1 Separatory Funnel,500-mL,4.2 Nessler Tubes,50-mL,4.3 Erlenmeyer Flask,125-mL,and4.4 Colorimeter or Turbidimeter,Method 2.5.Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all test.Unless otherwise indicated it is intended that allreagents shall conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Society,where such specification are available.2Other 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 halide-free distilled water.5.3 Chloride Standard(1 mL 0.0001 g Cl),Test Methods1,2,and 3Prepare by adding 0.165 g of sodium chloride(NaCl)to 1 L of halide-free distilled water.5.4 Chloride Standard(1 mL=0.000001 g Cl),TestMethod 4Dissolve 0.0660 g of sodium chloride in water anddilute to 1000 mL.Pipet 25 mL of this solution into a 1000-mLvolumetric flask,dilute to volume,and mix.5.5 Nitric Acid(sg gr 1.42),concentrated nitric acid(HNO3).5.6 Silver Nitrate Solution 0.1 NPrepare a 0.1 N solutionof silver nitrate(AgNO3).1These test methods are under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and are the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1,2015.Published June 2015.Originallyapproved in 1971.Last previous edition approved in 2010 as D2988 96(2010).DOI:10.1520/D2988-96R15.2Reagent 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.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.6.1 Prepare the silver nitrate solution by adding 16.99 g ofsilver nitrate to a 1-L volumetric flask and fill to the line withhalide-free distilled water.After shaking to dissolve theAgNO3,store in an amber bottle.5.7 Mercuric Acetate Solution,Test Method 4.5.7.1 Stock Mercuric Acetate SolutionDissolve 1.6 g ofmercuric acetate in 500 mLof water containing 3.5 mLof nitricacid.Dilute to 1000 mL and mix.5.7.2 Standard Mercuric Acetate SolutionDilute 40 mL ofstock mercuric acetate solution to 1000 mL and adjust the pHto 1.6 with nitric acid.Standardize in accordance with 7.5.5.5.7.3 s-Diphenylcarbazone Solution(Test Method 4)Dissolve 0.5 g of s-diphenylcarbazone in 100 mL of methanol.6.Hazards6.1 Solvent HazardsCo