Melting range á741ñ: between 37and 39.

Assay— When tested by thin-layer chromatography (see Chromatography á621ñ)with the use of plates coated with chromatographic silica gel mixture and a developing system consisting of a mixture of toluene and ethanol (9:1),examined under short-wavelength UVlight,a single spot is exhibited,with trace impurities.

Melting range á741ñ: between 172and 177.

Melting range,Class IIá741ñ: between 256and 260.

Specific rotation á781ñ: between +85and +88,determined in a solution in dioxane containing 75mg of equilenin in each 10mL.

Absorption maxima— An alcohol solution exhibits absorption maxima at 231,282,325,and 340nm.

Solubility— 200mg in 100mLof water yields a solution that remains clear and free from undissolved matter for 30minutes.

Loss on drying á731ñ— Dry it in vacuum over silica gel to constant weight:it loses not more than 2%of its weight.

Residue on ignition(Reagent test)— 0.5g,treated with 1mLof sulfuric acid and 2mLof nitric acid,yields between 42.0%and 44.0%of the dry weight (theory is 42.9%of Na2SO4).

Sensitiveness— Add 2mLof a solution (1in 1000)to 1mLof aluminum sulfate solution (1in 10,000),heat at 37±3for 5minutes,cool,and add 1mLof sodium acetate TS:a strong red to red-violet color is produced in not more than 5minutes.

Melting range á741ñ: between 118and 120.

Water,Method Iá921ñ: not more than 0.5%.

Residue on ignition á281ñ: not more than 0.1%.

Add the following:

Assay— Accurately weigh about 300mg,dissolve in 30mLof water,add phenolphthalein TS,and titrate with 0.1Nsodium hydroxide VS.Each mLof 0.1Nsodium hydroxide is equivalent to 11.013mg of C2H5SO3H:between 94.0%and 106.0%is found.

Refractive index á831ñ: between 1.432and 1.436at 20.

Peroxide— Transfer 8mLof potassium iodide and starch TSto a 12-mLground glass-stoppered cylinder about 15mm in diameter.Fill completely with the substance under test,mix,and allow to stand protected from light for 5minutes.No color develops.

Specific gravity á841ñ: about 0.93.

Boiling range(Reagent test)— Not less than 95%distills between 133and 135.

Assay— Dissolve about 50mg in 1mLof ether.Inject about 1µLof this solution into a suitable gas chromatograph (see Chromatography á621ñ)equipped with a flame-ionization detector and a 0.25-mm ×30-m capillary column containing stationary phase G1.The carrier gas is helium.The chromatograph is programmed as follows.Initially,the column temperature is equilibrated at 180,then the temperature is increased at a rate of 10per minute to 280,and maintained at 280for 10minutes.The injection port temperature is maintained at 280,and the detector is maintained at 300.The area of the 4¢-ethoxyacetophenone peak is not less than 97.5%of the total peak area.

Melting range á741ñ: between 34and 39.

Assay— Inject an appropriate specimen into a suitable gas chromatograph (see Chromatography á621ñ),helium being used as the carrier gas.The following conditions have been found suitable:a 3-mm ×2.4-m stainless steel column containing 20%phase G16on support S1A;the injection port,column,and detector temperatures are maintained at 180,195,and 250,respectively.The area of the ethyl benzoate peak is not less than 98%of the total peak area.

Refractive index á831ñ: between 1.5048and 1.5058at 20.

Specific gravity á841ñ: between 1.057and 1.062.

Acidity— Dissolve 2mLin 25mLof neutralized alcohol,add phenolphthalein TS,and titrate with 0.10Nsodium hydroxide:not more than 1.5mLis required to produce a pink color.

Assay— Transfer about 80mg,accurately weighed,to a suitable beaker,add 30mLof methanol,and dissolve by stirring.Slowly add 40mLof deionized water.[NOTE—If cloudiness appears when adding the deionized water,dissolve in 50mLof methanol only.]When solution is complete,titrate with 0.1Nsodium hydroxide VS,determining the endpoint potentiometrically.Perform a blank titration,and make any necessary correction.Each mLof 0.1Nsodium hydroxide is equivalent to 16.02mg of C7H12O4.Not less than 98.5%of C7H12O4is found.

Melting point á741ñ: between 101and 103.

Assay— Inject an appropriate specimen into a suitable gas chromatograph (see Chromatography á621ñ)equipped with a flame-ionization detector,helium being used as the carrier gas.The following conditions have been found suitable:a 0.25-mm ×10-m capillary column coated with a 1-µm layer of methylsilicone;the injection port temperature is maintained at 240;the detector temperature is maintained at 300;the column temperature is maintained at 150and programmed to rise 10per minute to 250.The area of the ethyl salicylate peak is not less than 99%of the total peak area.

Refractive index á831ñ: between 1.5216and 1.5236at 20.

Assay— Dissolve about 600mg,accurately weighed,in a mixture of 100mLof alcohol and 25mLof 1Mhydroxylamine hydrochloride in a beaker.Cover the beaker with a watch glass.Heat gently until condensate begins to form on the watch glass.Allow to cool for about 30minutes.Titrate with 0.5Nsodium hydroxide VS,determining the endpoint potentiometrically.Perform a blank determination,and make any necessary correction.Each mLof 0.5Nsodium hydroxide is equivalent to 67.09mg of C2H5C6H4CHO.Not less than 98%is found.

Add the following:

Boiling range(Reagent test): between 194and 200.

Residue on ignition— Evaporate 100mL(110g)in a tared evaporating dish over a flame until the vapors continue to burn after the flame is removed.Allow the vapors to burn until the specimen is consumed.Ignite at 800±25for 1hour,cool,and weigh:the residue weighs not more than 5.5mg (0.005%).

Acidity— Add 0.2mLof phenol red TSto 50mLof water,and titrate with 0.1Nsodium hydroxide to a red endpoint.Add 50mL(55g)of ethylene glycol,and titrate with 0.1Nsodium hydroxide:not more than 1mLis required to restore the red color (0.01%as CH3COOH).

Chloride(Reagent test)— A4.5-mL(5-g)portion shows not more than 0.025mg of Cl (5ppm).

Water,Method Iá921ñ: not more than 0.20%.

Melting range á741ñ: between 43and 47.

Assay— Dissolve about 290mg,accurately weighed,in 100mLof water,and add 10mLof glacial acetic acid.Titrate with 0.1Nsilver nitrate VS,determining the endpoint potentiometrically,using a silver-ion selective electrode and a calomel reference electrode containing 1Mpotassium nitrate.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nsilver nitrate is equivalent to 29.92mg of C12H14IN:not less than 97.0%is found.