ASTM_D_2760_-_70_1997.pdf

Designation:D 2760 70(Reapproved 1997)Standard Test Method forAnalysis of Sodium Triphosphate by the Simplified PaperChromatographic Method1This standard is issued under the fixed designation D 2760;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 is a single-step method2developed toreduce the analysis time for the determination of phosphatedistribution in condensed alkali phosphates where a separationof tripoly-and trimetaphosphate is desired.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.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water33.Summary of Test Method3.1 Separation of the various phosphate species in con-densed alkali phosphates is accomplished by ascending paperchromatography.The individual phosphate species are clearlyseparated in 60 to 75 min.The phosphorus in each of theseparated bands is determined colorimetrically,and the phos-phate ion distribution is calculated.4.Apparatus4.1 Battery Jar,cylindrical,8 in.(203 mm)in diameter by10 in.(254 mm)in height,with 10-in.diameter plate-glasscover.4.2 Chromatographic Spray Bottle,50-mL size.4.3 Spectrophotometer44.4 Filter Paper,special for paper chromatography,5in 9 by8-in.(229 by 203-mm)sheets.The necessary markings forthese sheets are shown in Fig.1.4.5 Micropipets,50-l capacity,with subdivisions at 10-lintervals.4.6 Pipet Filling Attachment,with screw control.64.7 Pipets,5-mL transfer.4.8 Pipet Filler74.9 Pipet,automatic,10-mL capacity.4.10 Platinum Wire,about 0.02 in.(0.5 mm)in diameter.4.11 Ultraviolet Lamp.4.12 Water Bath,consisting of a hot plate with several600-mL beakers.4.13 Refrigerator,maintained at 10C.5.Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.8Other 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 reagent water conformingto Specification D 1193.5.3 Ammonium Hydroxide(8 N)Mix equal volumes ofconcentrated ammonium hydroxide(NH4OH,sp gr 0.90)andwater.Adjust the concentration to 8.0 6 0.5 N.5.4 Ammonium Molybdate SolutionDissolve 50 g of am-monium molybdate(NH4)6Mo7O244H2O)in 450 mL ofwater.5.5 Chromatographic SolventDissolve 25 g of trichloro-acetic acid in water,add 1.75 mL of concentrated ammoniumhydroxide(NH4OH,sp gr 0.90)and dilute with water to 175mL.Add this to 325 mL of acetone and mix.This solvent canbe used for four papers only.Make fresh daily.1This method is under the jurisdiction of ASTM Committee D-12 on Soaps andOther Detergents and is the direct responsibility of Subcommittee D12.14 onAnalysis of Inorganic Alkaline Detergents.Current edition approved May 29,1970.Published July 1970.Originallypublished as D 2760 68.Last previous edition D 2760 68 T.2Based upon Karl-Kroupa,Editha,“Use of Paper Chromatography for Differ-ential Analysis of Phosphate Mixtures,”Analytical Chemistry,Vol 28,1956,p.1091;and Bernhard,D.N.,and Chess,W.B.,“Quantitative Evaluation of PaperChromatograms of Condensed Phosphate Mixtures,”Analytical Chemistry,Vol 31,1959,p.1026.3Annual Book of ASTM Standards,Vol 11.01.4ABeckman DU spectrophotometer has been found satisfactory for this purpose.5Schleicher&Schuell No.589.Orange Ribbon filter paper has been foundsatisfactory for this purpose.6A Scientific Glass catalog No.P-6628 attachment has been found satisfactoryfor this purpose.7A Will Corp.catalog No.22101 pipet filler has been found satisfactory for thispurpose.8Reagent 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.NOTICE:This standard has either been superseded and replaced by a new version or discontinued.Contact ASTM International(www.astm.org)for the latest information.5.6 Chromatographic SprayMix 25 mL of perchloric acid(HClO4,60 to 72%),5 mL of concentrated hydrochloric acid(HCl,