ASTM_D_1399_-_95_2000.pdf

Designation:D 1399 95(Reapproved 2000)Standard Test Method forUnsaponifiable Contents of Tricresyl Phosphate1This standard is issued under the fixed designation D 1399;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 covers the determination of the amountof unsaponifiable impurities in tricresyl phosphate.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.For specific hazardstatements,see Section 7.1.3 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water23.Summary of Test Method3.1 The specimen is refluxed in the presence of an aqueoussolution of sodium hydroxide which converts the phosphateester to water-soluble salts.The saponified material is extractedwith petroleum ether which dissolves any unsaponifiable orwater-insoluble material.The combined extracts are evapo-rated in a tared evaporating dish,and the residual nonvolatilematerial is determined.4.Significance and Use4.1 This test method determines the amount of unsaponifi-able impurities in tricresyl phosphate remaining after manu-facture or that may be introduced during handling and storage.4.2 Water-insoluble materials,which do not evaporate on asteam bath or in a drying oven operated at 75 6 5C for 1 h,will be included as unsaponifiable material.5.Apparatus5.1 Reflux Apparatus,consisting of a 250-mL Erlenmeyerflask equipped with a 24/40 standard-taper joint attached to anAllihn-type reflux condenser similarly equipped with a 24/40standard-taper joint.5.2 Separatory Funnel,having a capacity of 250 mL.5.3 Evaporating Dish,porcelain or glass,having a capacityof 120 mL.5.4 Steam Bath.5.5 Drying Oven,thermostatically controlled,at a tempera-ture of 75 6 5C.6.Reagents6.1 Purity of ReagentsUnless otherwise indicated,it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society,where such specifications are available.3Other-wise,the best available grade shall be used.6.2 Purity of WaterReferences to water shall be under-stood to mean reagent water conforming to Type IV ofSpecification D 1193.6.3 Petroleum Ether,having a boiling range from 30 to65C.6.4 Sodium Hydroxide(NaOH)Pellets.7.Hazards7.1 Tricresyl phosphate is hazardous through inhalation orskin absorption.Care should be taken in handling the material.7.2 Ortho-isomer of tricresyl phosphate is considered toxic.Trace amounts may be present in tricresyl phosphate speci-mens.8.Procedure8.1 Place approximately 30 mL of water in the 250-mLErlenmeyer flask and to this carefully add approximately 10 gof NaOH pellets.Carefully swirl the flask to dissolve theNaOH,and cool the solution to room temperature.8.2 By means of a weighing pipet,transfer a 10-g specimen,weighed to 1 mg,to the flask.Add several boiling-stones,connect the flask to the reflux condenser,and reflux for 1 h.(WarningSee 7.1 and 7.2.)8.3 At the end of the refluxing period remove the flask fromthe heat and wash the condenser down with 50 mL of water.8.4 Cool the flask to room temperature and transfer itscontent to the 250-mLseparatory funnel.Extract the saponified1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved Aug.15,1995.Published October 1995.Originallypublished as D 1399 56 T.Last previous edition D 1399 90.2Annual Book of ASTM Standards,Vol 11.01.3Reagent 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.1Copyright ASTM,100 Barr Harbor Drive,West Conshohocken,PA 19428-2959,United States.material three times with 25-mL portions of petroleum ether.Exercise particular care in separating the two phases so thatnone of the aqueous phase is occluded in the ether phase.8.5 Combine the ether extract and place in the 120-mLevaporating dish,weighed to 1 mg.Place on the steam bath andcarefully evaporate to dryness.Dry the bottom of the evapo-rating dish with a clean lint-free cloth and place in the dryingoven set at 75 6 5C for 1 h.Cool in a desiccator and weighthe evapora