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Pharmaceutical Chemistry: Instrumental Techniques PDF

788 Pages·1969·101.414 MB·English
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Pharmaceutical Chemistry Volume-2 Leslie G. Chatten Pharmaceutical Chemistry VOLUME 2 PharmaceuticarChemistry - EDITED BY LESLIEG. CHATIEN -PlitOIIUSOft Of 'HAItM'-C1l..,IC'-'l. C.H£MI.sU.Y hCt.'l.TY Of ,HAaMACY t.r."Ol'iU.SITY Of AU(ftTA ~. ALaOTA, CAl'IAOA va LiIME 2 Instrumental Tcc'b·nigw<. "';"({i. ~\\'.I~a/'('a ~ Proprielor Publisr,er, DisW,, l!l2~l;;~ re,arl seller of medical bO~ks Phone: 9660334, Mobile: 0172-049257 ._-, ._._ .... - -- -_. Pttmission 10 us.c portions of ~he lext of l.he ."a/iO#fal Fo,,,,,,kt,y. T .... ~lflh EditIon. ofTlcial September" L J96~_~has been gr:antec;t j»' the American Phannaa:utiaJ Associatiol\. The or Americ.ln Plu.rmaccutieal-Association is not rcspo:uibk r« any in.aQ;uracy quol.J.tion. or The: uw of ponions of the tt=xt the United StatCS Pharmacopeia X\'U Rt=\"ision. official September 1, J965. is by permission reo:jyed rrom Ihe Board of Trusl~s of the L'nited Slales Pharmac:orcial Co","'Cnlion. The said board is not responsible for any ilU.cC'uracics of the lexl thus UKd. The usc of portion~ of thc text of the Brilish Pha.nN.Copoc:la. J968, is made with the agreement of the General MediC31 Council. r COPYRIGHT '1; 1969 by MARCEL DEKKER, INC. ALL RIGHTS RESERVED . - 1/. No p.1-rt of this ..... ork may be reproduced 01" Ulili~d in any (orm or b)' any means. electronic or mechanical, includin, photoc:opyiD,. mtCrofilm. and fCQJrding. or hy any information stora~ aDd retrieval s)'Stem . .... ·ilhoUI 'permission in writing (rom the. pUblisher. MARCEL DEKKER. INC. ?S Madi~on Avenue! New Yorl, New York IOQI6 United Kingdom Edition puh/islJr-d b,l' ~ARCEL DEJ..:.KER LTD. 1-1 Crell/uri! }i"tC .\Iuidcll/lcad Vl'rI;·.Il1u. t:Ilt.:~lId .. , • Preface The incrC::lsin~ compk.1.11 u,:s \1( ph:lrm;l\:cU[h.::.t1 pn:par:ltions and th~ fn:.lrked cmph:.tsr:s on ljU:.thl~· l:ontr~11 by [hi.." cthH::.d manufac[Urer h3\'C' pbced J. greatcr load on the ingenUity of the control chemist. Such an individuJI must be so well tralneo that he is cap:Jblc of J.ppreciating the mefJ(S of the known techniques before selecting: tht: one: mpst suited to the task at hand. If established proccdures arc: not sUHable. the control cherrusl must be CJP:Jolc: of developing new methods. Thc:rdore. this nc .... and comprc:hensi .... c two· volume textbook on ph:lrmacc:ullcal Chemistry has b(cn wriuen for usc in the practie:ll training, of pharmacy students to enable them (0 take: their rightful place: in the ph:Jrmaceutical industry '~lnd in go'. . ernment bb0r:Horics concern~d ..... ith the 4uali(~· of medicin:.11 prc:parJ.tion~. T ..· .HS d~:.Jling "",ith analyticl! cheOlJ!:Itry that have ~e:n ""rinen !..:Ir and b~· :In:.l ytica I chemists do not, in gener;.al, adequately treat the: subject of .1nJ,lytic31 pharmaceutical chemistry. When one applies qu;lntitati .... e technique!. to the analyses of pharmaceutical dosage forms which, even in their sim?ies( srate, Jre compkx entities, one rr.ust I!mploy special considl!r:uions. Books on analytical Chemistry lack [hI! propa ~mphasis and suitJ.bk applications. Existing textbooks in pharm.Jceutical Chemistry . ..... hile considaing the p~J,rmace-utical aspects. ,often f.1il to tr~:H the subject in the de-pc:" which it deser\"es. This te.,' is meant to fulfill these needs. The editor. based upon his e:tperience with the Food and Drug Directorate vi the Government of Can:ldJ :IS ""l'"11 ;..IS his t"'aching of ph:lrrr.:1ceutical ..:hemlstr: "t the L:ni .. crslty of .-\lbcrLJ. lnJ the Cllntribut~-'rs. "r.,J. fllr [he most POJrt. 3rc all e.,!Xricnccd te:lchas of pharmaceutlc.J] chemiury or a rel.lted JI-iclpitne of ph:.lfmJ,cy. h.l\e ..:ons..-ious]y attempteJ to J.rri\·e .:H .J <\J,CI-ir:Jctvr:- blend of procedures In orl1c:r to pro\ldc :l bro:l..! b:Jiis on .... hJ(h the senior underg.r:lJu:lcc anl1 ~r:,dual(.' ~tul1cn[ can budd The f0("31 p.llnc of e,Kh ch;lpter i<;. thc prc~ent;H!On of the theor:-. PrJ..:!I":.J1 c:t.peo· m ..· nts h:l~c r.ccn ·carcfull\' sdccled io dcmonstr.J.lc :lll :lrrlic:ltlon of the thc0retlCll ":1)nsll.k"r:1tlOns.· Que!:llions JnJ problems. to.gcther ""jch .J. li~[ o~ references for suppkm. ent:u.v rC:,hJin":.! . h:.av.c. . bC_"'1.1 induded at t.he c.nd 01 Vi PREFACE Since the aim of this book is to provide a depth of understanding not evident in other books, it was decided to separate what is generally thought of as classical analytical techniques from those of instrumentation. The first volume, therefore, deals with theoretical and practical considerations of gravimetric andlysis,acid.basetitrimetry and pH, precipitation and complex formation, acidimetry and alkalimetry, nonaqucous titrimetry, compleo. metric analsis, nik.1cid1 assay. nthce!neous methods, ion exchange, chromatography, and the analysis of fixed and volatile oils. The second volume presents the theory and application of the foilo-vine instrumental techniques: visible and ultraviolet spectrophotometry, fluorescence photometry, turbidimetry and nephelometry, infrarcl Spectrophotometry and Raman spectroscopy, flame photometry and atomic absorption analysis, x-ray diffraction and optical Crystallography, mass spectromcwv, refractom- etry and interferometry, polarimetry and optical rotatory dispersion, gas chromatography, radioactivity, nuclear magnetic resonance, potentiornetric titrations and instrumental determination of pH, coulometrjc methods and chronopotentiometry, polarography, amperomctry, and conductance and high frequency. The editor is indebted to the various authors for their contributions. Their efforts are responsible for the quality.of this text. L.G.C. Contribl.ltors to Volume 2 JOH~ .-\ BILES. Ph.D. P"(lJ~':i5'Jr IIf PirtJrml1n. 5d,oo/ oj Phr.:r":t!t':. Cniufwy oj SlJuthCfII Caltj;)mia. Los .-I,,~!!I~J. California CA RY'fAS A. BUSS. Ph.D._ AJSocialr? PrO!c'JSor of Pharmacy. Col!(~'!f! 0/ Pharmacy. en;1( Fsity 0/ SCJskalChc' .. ~:an. Sarkutoon, SasJcalchl! ....· an A. CHISHOL~1.· D.Se .. Alftllyr:co/ R<!search. ·W",. S. :"'(uTell Co., Dinsion of RIcnardson"\{(,rull, Inc.. Cincinnati, Ohio ROSALD T. COLTTS. Ph.D .. Projr.'ssoT o[ Pltl1rml1UUlical CltL'lIrwry. [;"ifUJilY of Alberta, £Jlllonlon. Alberw STL"ART ERIKSE:-':, Ph.D .. Dirc'C(or, .\fL·dical Rr.'uarch. ,-Illergon PharmjJ· ceuticals. Stlr.ta Ana, Cali/ornia DAVID E. GLTT:\I.-\:", Ph.D .. Profusar oj Pharmauulics. School 0/ Pharmacy, SfOU Cnirusity of St'"'" York at Bu.tfaJo. Buffalo, S c'h' York J. GEORG E JEFFREY. Ph.D .. Projimor of Pif/ln,acy. Col/,!!, of pi,,,r.",uc,. CniL·t!rsiIY of SaJka(Che1Ian. Swkaroo/l. SQJkafC"~lIal/ PETER K..-\BASAK .. AUA:--':, Ph,D .. Physical & Analyucal Cheftl/CUI Reucrcn, Scheri,,! Corporarion, BloomfieM, ~\'''II" JUU,I" D. S. LAVERY. Ph, D., Lash ,'.!illa Chemical Laboratorin, CniarsilY of Toronlv, Toronto. Canada ROBERT .-\. LOCOCK, Ph.D, .1.SJISItJIIf p,oJ~'JsiJr 0/ Pha"':C("':l~:('al Cnt!,.:tstr.:, Fc("U!: .... 0/ Ph~rma(.~·, en;; c'lSil)" oj ...I/~ala. £dmoIlIOI:, .-Itbc!rrl1. Car.:Jda ~I.-\ THIAS P. ~IERTES, Ph D . .- IsJc)citJtt! Professor 0/ Pharmacy, Depart .. no'er.: t'/ .\/ ,·dICU:l1l Ch.',,':s:r.,·. School 0/ Pharmac." enil"(SIIY 0/ A"l1nJ·,:.I. Lal> '(r.c •• A"alTsoJ .-\:-.. TOI:-'" E;\ :--'OL·J.--\I \-1, Ph.D . .- Issvnalt' Pro/c'JJor of Pharmacy. FOC'..lIl., , tlf Pi:."n."cn . ('flU .'fJUX 0/ .-I1f·t!fla, Ed",onlon, A/be-no. C anoda • I'~e\/::-:: .l..!"::/:·n F.h,·..! JnJ O/US Dlr~r\'rJ.te. T.,rlJnll~. CJruJ.1 . .. '" Vjjj CONTRIBUTORS M. PERNAROWSKI Ph.D., Professor of Pl,arn,ac Facu/r) of P/7ar,,ic (Jnncr5jf of British Columbia Voncoucer, British Columbia E. A. ROBINSON Ph.D., Toronto, Toronto, canadAassociate Dean, Erinda/e college L;niiersj,1• of J. WB. RatOonB RINouSgOe.N L oPuhi.sDia.n, aProfessor o.[ hemjstr . Louisiana State UnherSj,t FRED T. SEMENIUK, Ph.D.., Professor of Pharmaceutical Chc#tjwri• School of Pharmacr, Uiirersj:' of North Carolina c/tape! Hill, North JOHN W. SHELL,1- Ph.D., Director of Research Allergan Pharmaceuticals, Santa Ana, Colfornja FRED W. TEARE, Ph.D., Associate Professor of Pharmaceutical C/:emis,rj Faculzi of Phorniacr, Unà-ersity of Toronto, Toronto, Ontario, Canada Present address: University of Kansas, Lawrence, Kansas. Contents of Volume 2 , vji CII:\YTER I Absorption Spectrop~otome~ry \1. ?ER:-J,.1o ROWSKI , LI Elcclrom:lgncllc RaJi:uion I.::! Ab~orpllon or RaJi:an( Energy 1.3 OU3nllt~Ii\"C Spc'Clrophol0n:t~try I) 1.-' f)C\'IJIICln\ (rtlm Deer" L.ly. " 1.5 Anal:o-,is or .\h:tlurn " 1.6 C""tlflmclt~· .I,I 1.7 Spo.."C13i ~kthoJs )9 1.8 SpcclropholomclC~rs and Colonmclcts Qucslkms H RcfcrcncC1 '6 CH .... PTER 2 InfrOlred Spectroscopy 59 ROSALD T. COt:TTS ,. 2.1 InlroduclLon Absorption Spcclroscop~ 6~ :.3 PhUrn.:lCCUlJc:a1 Applic3110ns of Inrr;ucd Spc..:::o:)Copy 108 R('r<:rcncC1o 125 ('"II ~rTER. J R;amOln Spectroscopy 127 E. r\. Rool.\;so:-.l Jnd D. S. LA\TRY .1.1 Inu.,.,jucl)\ln I." , 1.2 fhcon' • • ~-J.. .or:!8 .'.~ F 'po:r;mcIlI31 144 ).,l '\~rll':311\'n~ • 160 Q~c\I!llru 16) ~drrcn~("\ 164

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