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The Radiochemistry of Phosphorus

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The Radiochemistry of Phosphorus . .._ “5+6.a H75%4’ C.5 National Academy ““”v of Sciences ! National Research Council NUCLEAR SCIENCE SERIES The Radiochemistry of Phosphorus . I COMMlllEE ON NUCLEAR SCIENCE L.F.CUHTIM,Chd- HOBLliWD.EVANS,ViC#Ckal- N6ibndBureanofSbudar& MMU~ttn InatUubofTechdcsY J.A. DeJOHHN, .SwmItmy WeOUnglmussHleotrbCorpxntbn C.J.MMtK~ J.w.mvmx,JR. OakRidgeNatid I.mbOmtorg Mastiudts hBtiblb d TeohmlosY ROBERTG.COCWEAN E.D.KLEMA TaX8#AgriOultaualandMechaldd NorthwesternIJnlveralty collage W.WAYNBMSINKE SAMUELEP61’KIN Untvern[&ofMtuhlgna Cdlfomln hmtihrteofTeahmlc# J.J.NIC-N u.FANO MemorialHoaPlt4NewYork NatlandBureauofShndar& HOBBETI.PLATZMAN EHBBERTGO~ IahOlatdredeChimlePhyOiqw IUndearmvelopmemtcorponnon0! D.M. VAN PATTER Amarl13a BmtolEaseorahF~on LIAISONMEMBERS PAULC,.AEB~LD ~S K. REED Atomfo EnmsY Cammlmdon U.E.Ah Force J.HOWABDMo~ WILLIAME.WRIGHT NatlondSdem?aFoundation Ofbsd NavalRmenrah SUBCOMMlllEEON RADIOCHEMISTRY W,WAYNEMEINKS,Chairman EARLHYDE Unlv8r0i~ofMicblgnn Unlvmsi~.ofCdfomda(Berkeley) NATNANBALI.OU JUIJANNIEIAEN Nwd HxIIologlcalDefense Iabmalory HanfordIatarntc.fien GREQORYFLCHOPPIN G.DAVIDO’IOZLLEY PloritiStatsUntveraItg OakHidseNntlonalIahorntnry GEORGEA CCfWAN ELIJSP.STEINBERG I.DOAlamoaS4ientfficIabxatory ArEonneNation.dI.mlwrbry ARTHUHW,FAIRHALL PETERC.STEVENSON Ur&ersiWofWn9htrgbm Untveral&ofCdlfOrnln(Ltvermore) JEROMEHuDIS DUANEN,SUNDEHMAN BnmkhavmNauonnlLaboratory BaUd10MeumrldInstitita CONSULTANTS HERBERTM.CI.AHK JOHNW.WINCHESTER R&mluerPolytedmlcInstitute MamwtwettaJnsuhJwofTectmdc@y $wd. pq94r%p CHEMISTRY ..h C*5 The Radiochemistry of Phosphorus W. T. MULLINS and G. W. LEDDICOTTE Oak Ridge National Laboratory Oak Ridge, Tennessee IssuanceDate:?vlarch1962 LQs AIAMos scmNTIFxc LABORATORY MAY4-1962 ImmARIEs PROPERTY Subcommittee on Radiochemistry NationalAcademy of Sciences—National Research Council PrintedInUSA.Price$0.50.AvatlablefromtheOfficeofTed.mical Services,DeparbnentofCommerce,Washington25,D.C. FOREWORD The Subcommittee on Radlochem36try Is one of a number of subcommittees working under the Committee on Nuclear science within the National Academy of Sclencee - National Research council . Its members represent government, industrial, and university laboratories @ the areas of nuclear chemlBtry and analytical chemistry. The Subcommittee has concerned Itself with thoee areas of nuclear science which involve the chemist, such as the collec- tion and dlstrlbutlon of radlochemlcal procedures, the estab- lishment of speclf~catlons for radlochemically pure reagents, avallablllty of cyclotron tti for service irradiations, the place of radlochemlstry In the undergraduate college program, etc. This series of monographs has grown out of the need for up-to-date compilations of radlochemical tiformatlon and pro- cedures. The Subcommittee has endeavored to present a series which will be of maximum use to the workin&Bclentlst and which contains the latest available information. Each mono- graph collects in one volume the pertinent information required for radlochemlcal wark with en individual element or a group of closely related elements. An e~ert In the radlochemistry of the particular element haB written the monograph, following a standard format developed by the Subcommittee. The Atomic ”Energy Commieslon has spon60red the printing of the series. The Subcommittee is confident these publications will be useful not only to the radiochemist but also ,to the research worker in other fields such as physics, biochemistry or medictie who wlshee to use radlochemical techniques to solve a specific p~blem . W. Wayne Meinke, .Wizman Subcommittee on Radiochemistry 111 INTRODUCTION This volume which deals with the radlochemlatry of phosphorous is one of a series of monographs on radiochemlstry of the elements. There is Included a review of the nuclear and chemical features of particular interest to the radlochemlst , a discussion of prob- lems”of dissolution of a sample and counting techniques, and finally, a collection of radlochemlcal procedures for the element as found in the literature. The series of monographs will cover all elements for which radlochemlcal procedures are pertinent. Plans Include revision of the monograph periodically as new techniques and procedures warrant. The rehder is therefore encotiraged to call to the attention of the author any published cirunpublished materfal on the radlochemlstry of phosphorous which might be included In a re- vised version of the monograph. iv CONTENTS I. GeneralReferenceson the Inorganicand Analytical. Chemistryofphosphonla. 1 II. The RadioactiveNuclldesof l%osphoms . 1 The GeneralChemistryof phosphorus.. 2 A. ElementaryFnosphorue.. B. The chemical.Gm@uude of phosphorus. : 1. Reactiormwith Hydrogen.. 2. Reactionswith Oxygen.. 4 3. ReaCtiOIISwith ~ti. 6 k. Reaction5with the ~O@M . 6 5. Reactionswith Nitrogea.. 7 6. Reactionswith Metal~. 7 Iv. The AnalY-tid Chemistryof PhosphQrua. -I A. Separationby Precipitation.. 8 B. Separationby Electroly6ism. 9 c. Separationby Volatility. 9 l.).SolvsntExtractionSeptiona . 10 E. ChrWL9to17raDhicSePamtions. 10 1. With-In&nic-Adeofbent6. 10 2. By Ion ExchangeRestis . I-1 3. By Paper Cbmm3togmphy . I-1 v. Dissolutionof SamplesContainingphosphorus. 12 VI. &fe’qyRactices . 12 VII. CountingTechniquesfor the RadioactivePhoephorueIsotopes.. 13 VIII. RadiochemlcalProceduresfor the phosphorusFdlonuclldes. 13 References. ...%. 29 v The Radioch6mistry of Phosphorus W. T. MULLINS and G. W. LkDDIC@TE Oak Ridge National Laboratory* Oak Ridge, Tennessee I. GENERALREFERENCESON THE INoRGAmc AND ANALYTICALCHmImRY OF PHOSPHORUS Renw,H., Treatim on Inorgsmlc Chelmtry, Volume1, Elsevier, Ametedsm (1956). Kleinberg,J., Argersinger,W. J., Jr., and Griswold,E., bor”@nlc Chemistry,Heath,Boston (1960). Hilleb&nd,”W. F., Luudell,G. E. F., Bright,H. A., and Hoffman, J. L., ApplledInorgmic Analysis,JohnWiley and Sons,New York, 1958. Wilson,C. L.,“andWilson,D. W., ComprehensiveAnalyticalchemistry, Elaevier,hetemhu, 1959. Slenko,M. J., and Plane,“R.A., Cheroistqy,McGraw-EHU, New York, 1957. Ckrlot, G., and Bezier,D., @antltativeInorganicAndy ala, John Wiley and Sons,New York,.1957. Sidgwick,N. V., The Chemical.Elementsand Their Compounde,university Press,oxford,1951. Vea Wazer,J. R., Phosphome and Its cow und.e: VolumeI: Chemistzy, Intersclence,New York, 1958. Hutchh.eon,E., Chemistti- The Elementsand TheirReactions, Saunders,Pbiladelphla,1959. II. RADIOACTIVE~S OF PHOmORUS The radioactivenuclideaof phosphorusthat are of Interestin the rsdlo- chemistzyof phosphorusare .@venin Table I. Tbls tiblehas been coqlled *Operatedfor U. S. AtomicEnergyCommissionby Ubion CarbideCorporation. (1) ihum InformationappearingIn reportaby Strondnger,et al., and by I&he. Imd Harvey.(’) TABLE I . THE RADIOAGHVE NUCLIDFSOF PHOSPHORUS Radio- Half- Mode of Energyof ——nucllde 13fe = Radiation ProducedBy $9 4.6 s P+ Y 1.28,2.42 Si-p-n,Si-d-n,P-y-’n #o 2.55 m P+ p+ S.Labs Al-inn,Si-p-n,Si-He3-p, P-n-h, P-7-n,S-d-% C1-y-a,n Fe 14.3 d. P- @- 1.70 S5-d-y,Si-d-p,Si-He3-p P-d-p,P-n-7,S-n-p,S-d-a, Cl-n-a,C1-7-~n, Cl-d-pa ~33 25.4 d B- P- 0.2$ abO S-n-p, S-7-p,Cl-y-a p+ 1.2.4E B- P- 5.1, 3.2 S-n-p,Cl-n-a III. THE GEKEHAL_STRY OFPHOSPHORUS Phosphorusis neverfound in natureas the element. The Mef sources of phosphorusare phosphaterock,Ca (F04)2,and apatite,W2”3W3(F04)2. 3 Itis usuallyobtainedfrom these sourcesbyr&ing coke and m.ndwith the crushedrock or ore and heatjngthe mixturein an electficfurnace. Since the temperatureof the reactionIs”quitehigh, the phosphorusdistillsaway frau the reactlm~ and is tn3~ed and condensedunderwater as yellow or whitephosphorus. A. Elemen@y Fhos@mle phosphorusexistsh at leastthreeallotropicforma. The white phos- phorus (or yellowphosphorus,if it is hpure) obtitiedby a titillation of phcmphoruehas a nmltingpoint of 4h°C.It dissolvesin organicliquids, crya~~zes h the cubicform,and burns spontaneouslyin air. When heated in the absenceof air to a tempe=+mxe of 250° C, it is convertedto red phosphorus. The colorand physicalpropertiesof red phosphorus depe&ieupen the temperatureand the lengthof the heatingpetibd.” It ui.12cryetdJlze in the rhoniboh~ fozm,and it is stablein air at room temperatllm.Red phoephozueIs insolublein organicIlquids. A b@ck allotropicform of phoephorueIs obtainedby heatingwhlte phoaphoms at 200° C and at a FJ.=ssm of about13,000aizuospheres.It Is rhombohednd in form and is a &ad ele’i+cricalconductor.Black phosphoruscanbe convertedto red phosphorusby heatingat &rperatures above 500°. B. The ChemicalConP3undsOf Phcmphorue Tho~phorusexhibitsoxidationet%tesOf -3, -2, +1, +2, +3, +4, and +5. The principleoxidationstateof phosphorus1S +5; however,+3 cm- poundeare not uncommon. Phosphoruscan form compmnds ulth hydrogen,oxygen, m.dfur,the halogens,and nitrogen. It can reactwith certainmetalEto form phosphides. Table II liEtsmany of the phosphoruscompcmndeand givesinfor- mationon their solublli~ in water and otheragents. Some geneml ll&onm- tion abouttheeeand otherphoephoruecompouudeis @ven below. More specific informationhae been given in reviewsby Vsm Wazer‘3) and Hutcldneon.(4) mm. sOlubiutvOfPllamc~ Sol*lain(sls,m~maakwrln SOlllbl.einether, ham, cblOrO— *, a32mrldccl~ ~inaadmlmndadd Ir9dmlla 3 1. Reactionswith Hydrown The hydrogencompoundsof phosphome cannotbe preparedby a direct uuion of the elements. Phospbine,PH~, ~ ~P~EPMne, “p2H4,Sre USUdW fonnedby heatingvbitephosphorusin the presenceof aqueoussodiumhydrotide or by hydrolyzingaluminumphospbidewith m.dfuricacid. PH3 ip extremely volatileand is &l.aumble In air. Phosphinela a toxic compoundand la conBide&blylese
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