Insoluble matter(Reagent test): not more than 1mg,from 20g (0.005%).

Chloride(Reagent test)— One g shows not more than 0.01mg of Cl (0.001%).

Sulfate(Reagent test,Method II)— Dissolve 10g in 100mLof water,add 1mLof hydrochloric acid,and filter:the residue weighs not more than 1.2mg more than the residue obtained in a complete blank test (0.005%).

Substances not precipitated by hydrogen sulfide— Dissolve 2g in a mixture of 135mLof water and 15mLof 1Nsulfuric acid,heat to boiling,and pass a rapid stream of hydrogen sulfide through the solution as it cools.Filter,and to 75mLof the clear filtrate add 0.25mLof sulfuric acid,then evaporate to dryness,and ignite gently:the residue weighs not more than 1mg (0.1%).

Insoluble matter (Reagent test): not more than 1mg,from 20g (0.005%).

Chloride (Cl )(Reagent test)— One g shows not more than 0.01mg of Cl (0.001%).

Sulfate(Reagent test,Method II)— Evaporate a mixture of 12g of specimen and 25mLof hydrochloric acid on a steam bath to dryness.Add another 15mLof hydrochloric acid,and again evaporate to dryness.Dissolve the residue in 100mLof water,filter,and add 1mLof hydrochloric acid:the residue weighs not more than 1.0mg more than the residue obtained in a blank test (0.003%).

Copper (Cu)— Dissolve 0.5g in 10mLof water,add 10mLof Ammonium Citrate Solution(see Lead á251ñ),and adjust the reaction of a pHof about 9by the addition of 1Nammonium hydroxide (about 30mL).Add 1mLof sodium diethyldithiocarbamate solution (1in 1000),and mix.Add 5mLof amyl alcohol,shake for about 1minute,and allow the layers to separate:any yellow color in the amyl alcohol layer is not darker than that of a blank to which 0.01mg of Cu has been added (0.002%).

Iron(Fe)— Dissolve 1g in 15mLof water,add 2mLof hydrochloric acid,and boil for 2minutes.Cool,and add about 30mg of ammonium persulfate and 15mLof a solution of potassium thiocyanate in normal butyl alcohol (made by dissolving 10g of potassium thiocyanate in 10mLof water,warming the solution to about 30,diluting with normal butyl alcohol to 100mL,and shaking until clear).Shake vigorously for 30seconds,and allow the layers to separate:any red color in the clear alcoholic layer is not darker than that of a blank to which 0.01mg of Fe has been added (0.001%).

Lead(Pb)— Dissolve 1.0g in 10mLof water,add 0.2mLof glacial acetic acid,and filter if necessary.To a 7-mLportion of water add 0.2mLof glacial acetic acid and 3mLof Standard Lead Solution(see Lead á251ñ),and mix,to provide a blank.Then add to each solution 1.0mLof potassium chromate solution (1in 10),and mix:after 5minutes,the test solution is not more turbid than the blank (0.003%).

Substances not precipitated by hydrogen sulfide— Dissolve 2g in 145mLof water,add 5mLof sulfuric acid (1in 10),heat to boiling,and pass a rapid stream of hydrogen sulfide through the solution as it cools.Filter,and to 75mLof the clear filtrate add 0.25mLof sulfuric acid,then evaporate to dryness,and ignite gently:the residue weighs not more than 1mg (0.1%).

Residue on ignition(Reagent test)— Ignite 5g at 550:the residue weighs between 150and 300mg (3.0%to 6.0%).

Calcium— Treat the residue from the preceding test with 10mLof diluted hydrochloric acid,filter,and to the clear filtrate add 5mLof ammonium oxalate TS:it shows a white precipitate upon standing.

Loss on drying á731ñ— Dry it in vacuum at 70to constant weight:it loses not more than 7.0%of its weight.

Fat— Suspend 1.0g in 5mLof alcohol in a Mojonnier flask,add 0.8mLof stronger ammonia water and 9mLof water,and shake.Add a second 5-mLportion of alcohol,then add successive portions of 25mLeach of ether and solvent hexane,shaking after each addition by inverting the flask 30times.Centrifuge,decant the solvent layer,evaporate it at a low temperature,and dry on a steam bath:the residue weighs not more than 20mg (2.0%).

Nitrogen content,Method Iá461ñ— Between 12.5%and 14.3%of Nis found,calculated on the anhydrous basis.

Suspensibility in water— Place 2g in a beaker,and add cool water slowly with stirring to form a thin,smooth paste.Add additional water to make a total of 100mL.Stir,and heat to 80:a milky suspension is formed that does not settle after standing for 2hours.

Assay— Accurately weigh about 400mg of the salt,previously dried at 150to constant weight,and transfer to a 250-mLbeaker.Dissolve the test specimen in 150mLof water containing 2mLof 3Nhydrochloric acid,add 15mLof 1Nsodium hydroxide and 250mg of hydroxy naphthol blue,and titrate with 0.05Medetate disodium VSuntil the solution turns deep blue in color.Each mLof 0.05Medetate disodium is equivalent to 8.307mg of Ca3(C6H5O7)2:between 97.5%and 101%is found.

Calcium oxide and carbonate— Triturate 1g of calcium citrate with 5mLof water for 1minute:the mixture does not turn red litmus blue.Then add 5mLof warm 3Nhydrochloric acid:only a few isolated bubbles escape.

Hydrochloric acid-insoluble matter— Dissolve 5g by heating with a mixture of 10mLof hydrochloric acid and 50mLof water for 30minutes:not more than 2.5mg of insoluble residue remains (0.05%).

Loss on drying á731ñ— Dry it at 150to constant weight:it loses between 12.2%and 13.3%of its weight.

Arsenic á211ñ— Proceed with 0.50g as directed for organic compounds (6ppm of As).

Heavy metals,Method Iá231ñ: 0.002%.

Assay— Accurately weigh about 500mg,previously dried at 120for 4hours,transfer to a suitable container,and dissolve in 150mLof water containing 2mLof diluted hydrochloric acid.Add 15mLof sodium hydroxide TSand 300mg of hydroxy naphthol blue indicator,and titrate with 0.05Medetate disodium VSuntil the solution is deep blue in color.Each mLof 0.05Medetate disodium is equivalent to 10.91mg of C6H10CaO6.Not less than 98%is found.

Loss on drying á731ñ— Dry it at 120for 4hours:it loses between 25.0%and 30.0%of its weight.

Acidity— Add phenolphthalein TSto 20mLof a 1in 20solution,and titrate with 0.10Nsodium hydroxide:not more than 0.50mLis required to produce a pink color.

Heavy metals(Reagent test)— Dissolve 1g in 2.5mLof diluted hydrochloric acid,dilute with water to 40mL,and add 10mLof hydrogen sulfide TS:any brown color produced is not darker than that of a control containing 0.02mg of added Pb (0.002%).

Magnesiumand alkali salts— Mix 1g with 40mLof water,carefully add 5mLof hydrochloric acid,heat the solution,boil for 1minute,and add rapidly 40mLof oxalic acid TS.Add immediately to the warm mixture 2drops of methyl red TS,then add ammonia TSdropwise,from a buret,until the mixture is just alkaline.Cool to room temperature,transfer to a 100-mLgraduated cylinder,dilute with water to 100mL,mix,and allow to stand for 4hours or overnight.Filter,and transfer to a platinum dish 50mLof the clear filtrate,to which has been added 0.5mLof sulfuric acid.Evaporate the mixture on a steam bath to a small bulk.Carefully heat over a free flame to dryness,and continue heating to complete decomposition and volatilization of ammonium salts.Finally ignite the residue at 800±25for 15minutes:the residue weighs not more than 5mg (1%).

Volatile fatty acid— Stir about 500mg with 1mLof sulfuric acid,and warm:the mixture does not emit an odor of volatile fatty acid.

Melting range á741ñ: decomposes at about 199.

Assay— Inject an appropriate sample dissolved in acetone into a gas chromatograph (see Chromatography á621ñ)that is equipped with a flame-ionization detector and contains a 0.53-mm ×30-m capillary column coated with a layer of phase G25.The carrier gas is helium,flowing at a rate of 9mLper minute.The chromatograph is programmed as follows.Initially the column temperature is equilibrated at 150,then the temperature is increased at a rate of 10per minute to 250.The injection port temperature is maintained at 240,and the detector temperature at 265.The area of the capric acid peak is not less than 98.5%of the toal peak area.

Melting range á741ñ: between 30and 33.

Assay— Inject an appropriate volume into a 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 ×30-m capillary column coated with a 1-µm layer of phase G2;the injection port temperature is maintained at 280;the detector temperature is maintained at 300;and the column temperature is maintained at 280.The area of the C12H9Npeak is not less than 95.5%of the total peak area.

Measuring range: 0.01to 0.3Vol.–%.

Measuring range: 5to 150ppm.

Residue on ignition (Reagent test)— Ignite 2g:the residue weighs not more than 20mg (1.0%).

Loss on drying á731ñ— Dry it at 105to constant weight:it loses not more than 10.0%of its weight.

Alkalinity— Shake 1g with 20mLof water for 10minutes,and filter:the filtrate is not alkaline to red litmus paper.

Soluble substances— When the filtrate from the Alkalinitytest is evaporated and dried at 105,the residue weighs not more than 1mg (0.1%).

Fats— Dissolve 1g in a mixture of 10mLof water and 5mLof alcoholic ammonia TS,and shake out with two 20-mLportions of solvent hexane.Evaporate the hexane at a low temperature,and dry at 80:the weight of the residue does not exceed 5mg (0.5%).

Nitrogen content,Method Iá461ñ: between 15.2%and 16.0%of Nis found,on the anhydrous basis.

Melting range á741ñ: between 104and 105.

Residue on ignition(Reagent test)— Ignite 500mg with 5drops of sulfuric acid:the residue weighs not more than 1mg (0.2%).

Moisture content of fully regenerated and expanded resin— Transfer 10to 12mLof the resin (as received)to a flask,and convert it completely to the hydrogen form by stirring with 150mLof hydrochloric acid solution (5in 100)for not less than 30minutes.Decant the acid,and wash the resin in the same manner with water until the wash water is neutral to litmus (pH3.5).

Total wet volume capacity— Transfer 3to 5mLof the regenerated,undried (see Moisture contentabove)resin to a 5-mLgraduated cylinder,and fill it with water.Remove any air bubbles from the resin bed with a stainless steel wire,and settle the resin to its minimum volume by tapping the graduated cylinder.Record the volume of the resin.

Wet screen analysis— The purpose of this test is to properly identify the mesh size of the resin.To obtain an accurate screen analysis would require special apparatus and technique.

Assay— Weigh accurately about 800mg,transfer to a flask,add 25mLof water and 3mLof sulfuric acid,and warm until dissolved.Cool,and add 60mLof a mixture of 1volume of phosphoric acid and 20volumes of water.Add 25mLof potassium iodide solution (1in 10),insert the stopper in the flask,and allow to stand for 15minutes.Replace the air over the solution with carbon dioxide,and while continuing the flow of carbon dioxide into the flask,titrate the liberated iodine with 0.1Nsodium thiosulfate VS,adding 3mLof starch TSas the endpoint is approached.Each mLof 0.1Nsodium thiosulfate is equivalent to 33.22mg of Ce(SO4)2.Not less than 80.0%is found.

Chloride(Reagent test)— Dissolve 1g in a mixture of 5mLof nitric acid and 4mLof water.Filter,if necessary,and dilute with water to 20mL.To 10mLof the dilution add 1mLof silver nitrate TS,allow to stand for 10minutes,and filter until clear.To the remaining 10mLof test solution add 1mLof silver nitrate TS:any turbidity produced does not exceed that in a control prepared by adding 0.05mg of Cl to the filtrate obtained from the first 10mLof test solution (0.01%).

Heavy metals— Heat 500mg with a mixture of 10mLof water and 0.5mLof sulfuric acid until solution is complete.Cool,dilute with water to 50mL,and bubble hydrogen sulfide gas through the solution until it is saturated:the precipitate that is formed is white or not darker than pale yellow.

Iron— Dissolve 100mg in a mixture of 5mLof water and 2mLof hydrochloric acid,warming if necessary,and cool.Transfer to a glass-stoppered cylinder,dilute with water to 25mL,and add 5mLof ammonium thiocyanate TSand 25mLof ether.Shake gently,but well,and allow the layers to separate:any pink color in the ether layer is not darker than that of a control,similarly prepared,containing 0.02mg of added Fe (0.02%).

Adsorptive power— Dissolve 100mg of strychnine sulfate in 50mLof water,add 1g of the test specimen,shake during 5minutes,and filter through a dry filter,rejecting the first 10mLof the filtrate.To a 10-mLportion of the subsequent filtrate add 1drop of hydrochloric acid and 5drops of mercuric iodide TS:no turbidity is produced.

Residue on ignition(Reagent test)— Ignite 500mg:the residue weighs not more than 20mg (4.0%).

Reaction— Boil 2g with 50mLof water for 5minutes,allow to cool,restore the original volume by the addition of sufficient water,and filter:the filtrate is colorless and is neutral to litmus paper.

Acid-soluble substances— Boil 1.0g with 25mLof dilute hydrochloric acid (1in 5)for 5minutes,filter into a tared porcelain crucible,and wash the residue with 10mLof hot water,adding the washings to the filtrate.To the combined filtrate and washings add 1mLof sulfuric acid,evaporate to dryness,and ignite to constant weight:the residue weighs not more than 35mg (3.5%).

Alcohol-soluble substances— Boil 2g with 40mLof alcohol for 5minutes under a reflux condenser,and filter.Evaporate 20mLof the filtrate on a steam bath,and dry at 105for 1hour:the residue weighs not more than 2mg (0.2%).

Uncarbonized constituents— To 250mg add 10mLof sodium hydroxide TS,heat to boiling,and filter:the filtrate is colorless.

Chloride(Reagent test)— A5-mLportion of the filtrate obtained in the test for Reactionshows not more than 0.04mg of Cl (0.02%).

Sulfate(Reagent test,Method I)— A5-mLportion of the filtrate from the test for Reactionshows not more than 0.3mg of SO4(0.15%).

Sulfide— Place 1g in a small flask with a narrow neck,add 35mLof water and 5mLof hydrochloric acid,and boil gently:the escaping vapors do not darken paper moistened with lead acetate TS.

Assay— When tested by thin-layer chromatography,with the use of plates coated with chromatographic reversed-phase C18mixture,a developing system consisting of 1Nacetic acid in methanol and 1Nacetic acid (19:1),and sprayed with a mixture of sulfuric acid and methanol (1:1),heated at 110for 20minutes,and examined visually and under long-wavelength UVlight,a single spot is exhibited.

Melting range á741ñ: between 165and 168.

Measuring range: 0.2to 3ppm.

Assay—

Melting range á741ñ: between 79and 80.

Solubility— One g dissolves in 30mLof alcohol to form a clear solution.

Melting range á741ñ: between 178and 181.

Residue on ignition(Reagent test): not more than 0.1%.

Assay— Inject an appropriate volume into a 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 ×30-m capillary column coated with a 1-µm layer of phase G2;the injection port temperature is maintained at 250;the detector temperature is maintained at 300;and the column temperature is maintained at 150and programmed to rise 10per minute to 280.The area of the C10H15Cl peak is not less than 97.5%of the total peak area.

Assay— Inject an appropriate specimen into a 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 ×30-m capillary column coated with a 1-µm layer of phase G2;the injection port temperature is maintained at 250;the detector temperature is maintained at 300;and the column temperature is maintained at 150and programmed to rise 10per minute to 280.The area of the C6H6ClNpeak is not less than 99%of the total peak area.

Refractive index á831ñ: between 1.592and 1.596at 20.

Assay— Dissolve about 700mg,accurately weighed,in a mixture of 100mLof hot alcohol and 50mLof water.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 78.28mg of ClC6H4COOH.Not less than 98%is found.

Solubility— One g dissolved in 25mLof 0.5Nsodium hydroxide yields a clear and complete solution.

Assay— Inject an appropriate specimen into a 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 ×30-m capillary column coated with a 1-µm layer of a phase consisting of 14%cyanopropylphenyl-86%dimethylpolysiloxane;the injection port temperature is maintained at 150;the detector temperature is maintained at 300;and the column temperature is maintained at 50and programmed to rise 10per minute to 200.The area of the C2H6ClN·HCl peak is not less than 99%of the total peak area.

Melting range á741ñ: between 150and 246.

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 butyl alcohol,water,and acetic acid (60:25:15),and examined under short-wavelength UVlight,a single spot is exhibited,with trace impurities.

Assay— Use a gas chromatograph equipped with a flame-ionization detector.The following conditions have been found suitable:a 3.2-mm ×1.83-m stainless steel column is packed with 7%phase G2on support S1A;the injection port temperature is maintained at 250and the detector at 310;and the column temperature is programmed to increase at a rate of 10per minute from 50to 250.Not less than 90%of C10H7Cl is found,of which not more than 10%is 2-chloronaphthalene.

Refractive index á831ñ: between 1.6320and 1.6340,at 20.

Assay— Inject an appropriate volume into a 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 ×30-m capillary column coated with a 1-µm layer of phase G2;the injection port temperature is maintained at 280;the detector temperature is maintained at 300;and the column temperature is maintained at 180and programmed to rise 10per minute to 280.The area of the C6H4ClNO2peak is not less than 98%of the total peak area.

Melting range á741ñ: between 107and 109.

Assay— Transfer about 200mg,accurately weighed,to a 100-mLbeaker,add 25mLof water,swirl to dissolve,and cautiously add,dropwise,sufficient sodium hydroxide solution to ensure complete solution of the specimen.Transfer the solution to a glass-stoppered,500-mLflask,using water to rinse the beaker,and dilute with water to about 100mL.Add 25.0mLof 0.1Npotassium bromide-bromate VSand 10mLof hydrochloric acid,immediately insert the stopper in the flask,and swirl vigorously for 2to 3minutes.Remove the stopper,quickly add 5mLof potassium iodide solution (1in 5),taking care to avoid loss of bromine,immediately insert the stopper in the flask,and shake thoroughly for about 1minute.Remove the stopper,rinse it and the neck of the flask with water,and then titrate with 0.1Nsodium thiosulfate VS,adding 3mLof starch TSas the endpoint is approached.Each mLof 0.1Npotassium bromide-bromate consumed is equivalent to 6.43mg of C6H5OCl.Not less than 99%is found.

Melting range á741ñ: between 42and 44.

Boiling range (Reagent test)— Not less than 90%distils between 218.5and 221.5.

Assay— Inject an appropriate volume into a 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 ×30-m capillary column coated with a 1-µm layer of phase G2;the injection port temperature is maintained at 230;the detector temperature is maintained at 300;and the column temperature is maintained at 130and programmed to rise 10per minute to 280.The area of the C6H5ClOpeak is not less than 99.0%of the total peak area.

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 cyclohexane,chloroform,and acetic acid (14:4:2),and examined visually and under long-wavelength UVlight or iodine spray,a single spot is exhibited.

Melting range á741ñ: between 172and 178.

Caution—It reacts vigorously with water,alcohols,and other hydrogen donors.Store in tight glass containers.

Refractive index á831ñ: between 1.3850and 1.3890at 20.

Assay— Transfer about 100mg,previously dried at 105for 2hours and accurately weighed,to a beaker,add 20mLof water and 1drop of aluminum chloride solution (1in 10),and mix.Add,slowly,20mLof a freshly prepared,filtered sodium tetraphenylborate solution (1in 50),and allow the mixture to stand for 30minutes with occasional swirling.Filter through a medium-porosity,sintered-glass filter,and wash the beaker and the precipitate with four 10-mLportions of water.The weight of the precipitate,determined after drying at 105for 2hours,and multiplied by 0.3298,gives the equivalent weight of C5H14ClNO.Not less than 99.5%is found.

Residue on ignition á281ñ: not more than 0.1%.

Assay— Dissolve about 125mg,accurately weighed,in 50mLof glacial acetic acid.Add a few drops of p-naphtholbenzein TSand titrate with 0.1Nperchloric acid VS.Perform a blank determination and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 14.72mg of C19H22N2O.Not less than 99.0%is found.

Loss on drying á731ñ— Dry it at 105to constant weight:it loses not more than 1.0%of its weight.

Melting range á741ñ: between 200and 205.

Specific rotation á781ñ: between -105and -115,calculated on the dried basis,determined in a solution in alcohol containing 10mg per mL.

Assay— Dissolve about 125mg,accurately weighed,in 50mLof glacial acetic acid.Add a few drops of p-naphtholbenzein TSand titrate with 0.1Nperchloric acid VS.Perform a blank determination and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 14.72mg of C19H22N2O.Not less than 99.0%is found.

Loss on drying á731ñ— Dry it at 105to constant weight:it loses not more than 1.0%of its weight.

Melting range á741ñ: between 255and 261.

Specific rotation á781ñ: between +219and +229,calculated on the dried basis,determined in a solution in alcohol containing 50mg per 10mL.

Absorptivity— Its absorptivity at 275nm,in alcohol solution,is about 1700.

Loss on drying á731ñ— Dry it at 105for 4hours:it loses not more than 3.0%of its weight.

Residue on ignition— Accurately weigh about 1g,previously dried at 105for 4hours,and place it in a porcelain dish or crucible.Ignite carefully until well charred,cool,add 2mLof sulfuric acid,and carefully ignite until the residue is white or practically so.Cool,add 0.5mLof sulfuric acid and 1mLof nitric acid,evaporate,and again ignite to constant weight:the weight of the sodium sulfate so obtained is between 20.0%and 24.0%of the weight of the dried specimen taken.

Sensitiveness— To 50mLof carbon dioxide-free water add 0.1mLof congo red solution (1in 1000).The red color of the solution is changed to violet by the addition of 0.05mLof 0.10Nhydrochloric acid and is restored by the subsequent addition of 0.05mLof 0.10Nsodium hydroxide.

Absorption maximum— The UVabsorption spectrum of a 1in 100,000solution in alcohol shows a maximum at about 238nm.

Specific rotation á781ñ: about +209,determined in a 1in 100solution in alcohol.

Chloride(Reagent test)— One g shows not more than 0.02mg of Cl (0.002%).

Substances not precipitated by hydrogen sulfide— Determine as directed for ACSreagent grade of Cupric Acetate:the residue weighs not more than 6mg (0.15%).

Assay— Dissolve about 300mg,accurately weighed,in 25mLof water and 25mLof alcohol.Titrate with 0.1Nsodium hydroxide VS,determining the endpoint potentiometrically.Perform a blank determination and make any necessary corrections.Each mLof 0.1Nsodium hydroxide is equivalent to 85.06mg of C3H3NO2.Not less than 99%is found.

Solubility— Separate 1-g portions dissolve completely in 10mLof water and in 10mLof alcohol,respectively,to yield colorless solutions.

Assay— When examined by gas-liquid chromatography,using suitable gas chromatographic apparatus and conditions,it shows a purity of not less than 98%.

Add the following:

Specific rotation á781ñ: between -215and -225,determined in a 2in 100solution of test specimen,previously dried over silica gel for 4hours,in dilute hydrochloric acid (1in 10)at a temperature of 20.

Loss on drying á731ñ— Dry it over silica gel for 4hours:it loses not more than 0.2%of its weight.

Residue on ignition (Reagent test): not more than 0.1%.