ASTM_E_1584_-_11.pdf

Designation:E158411Standard Test Method forAssay of Nitric Acid1This standard is issued under the fixed designation E1584;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.1.Scope1.1 This test method covers determination of the assay ofnitric acid by total acidity.This test method is suitable forconcentrations between approximately 50 and 70%,calculatedas nitric acid.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 Review the current Material Safety Data Sheets(MSDS)for detailed information concerning toxicity,first aidprocedures,and safety precautions.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 8.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E200 Practice for Preparation,Standardization,and Storageof Standard and Reagent Solutions for Chemical AnalysisE300 Practice for Sampling Industrial Chemicals3.Summary of Test Method3.1 Aweighed sample of acid is diluted in water and titratedwith 1.0 N sodium hydroxide solution,using phenolphthaleinas the end-point indicator.4.Significance and Use4.1 This test method provides a means for assaying nitricacid,based on total acidity.The concentration of nitric acid isimportant in many of the uses of nitric acid,includingspecification compliance and manufacturing control.5.Interferences5.1 Acids other than nitric,and compounds that consumesodium hydroxide,will yield erroneously high results.6.Apparatus6.1 Erlenmeyer Flask,250 mL,glass stoppered.6.2 Buret,50 mL,Class A.NOTE1A digital buret capable of measuring volumes to the nearest0.01 mL may be used in place of a conventional buret.7.Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Type II or Type III of Specification D1193.7.3 Phenolphthalein Indicator Solution(10 g/L)Dissolve1 g of phenolphthalein in 100 mL of ethanol(95%),methanol,or isopropanol.51This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicalsand is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved Aug.1,2011.Published September 2011.Originallyapproved in 1993.Last previous edition approved in 2005 as E1584 00(2005)1.DOI:10.1520/E1584-11.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Reagent 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.5This reagent is also described in Practice E200.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.4 Sodium Hydroxide,Standard Solution(1.0 N)Prepareand standardize in accordance with Practice E200,remember-ing to record the temperature of the NaOH solution during thestandardization to the nearest C.NOTE2Because of atmospheric CO2absorption by NaOH,1.0 NNaOH solutions will need frequent standardization.8.Safety Precautions8.1 Nitric acid is dangerous if handled improperly.It is astrong corrosive acid and a strong oxidizer.Contact with othermaterial may cause fire.Avoid inhalation of fumes or mist andany contact with skin or eyes.8.2 Clean up all spills immediately by covering the spillwith vermiculite or some other inert absorbent material andsweeping it into a pan.Dispose of the vermiculite by floodingwith water and